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Item 2D metal carbides and nitrides (MXenes) for energy storage(Nature Publishing Group, 2017-01-17) Anasori, Babak; Lukatskaya, Maria R.; Gogotsi, Yury; Mechanical Engineering and Energy, School of Engineering and TechnologyThe family of 2D transition metal carbides, carbonitrides and nitrides (collectively referred to as MXenes) has expanded rapidly since the discovery of Ti3C2 in 2011. The materials reported so far always have surface terminations, such as hydroxyl, oxygen or fluorine, which impart hydrophilicity to their surfaces. About 20 different MXenes have been synthesized, and the structures and properties of dozens more have been theoretically predicted. The availability of solid solutions, the control of surface terminations and a recent discovery of multi-transition-metal layered MXenes offer the potential for synthesis of many new structures. The versatile chemistry of MXenes allows the tuning of properties for applications including energy storage, electromagnetic interference shielding, reinforcement for composites, water purification, gas- and biosensors, lubrication, and photo-, electro- and chemical catalysis. Attractive electronic, optical, plasmonic and thermoelectric properties have also been shown. In this Review, we present the synthesis, structure and properties of MXenes, as well as their energy storage and related applications, and an outlook for future research.Item 2D MXenes: Tunable Mechanical and Tribological Properties(Wiley, 2021-04-28) Wyatt, Brian C.; Rosenkranz, Andreas; Anasori, Babak; Mechanical and Energy Engineering, School of Engineering and Technology2D transition metal carbides, nitrides, and carbonitrides, known as MXenes, were discovered in 2011 and have grown to prominence in energy storage, catalysis, electromagnetic interference shielding, wireless communications, electronic, sensors, and environmental and biomedical applications. In addition to their high electrical conductivity and electrochemically active behavior, MXenes' mechanical properties, flexibility, and strong adhesion properties play crucial roles in almost all of these growing applications. Although these properties prove to be critical in MXenes' impressive performance, the mechanical and tribological understanding of MXenes, as well as their relation to the synthesis process, is yet to be fully explored. Here, a fundamental overview of MXenes' mechanical and tribological properties is provided and the effects of MXenes' compositions, synthesis, and processing steps on these properties are discussed. Additionally, a critical perspective of the compositional control of MXenes for innovative structural, low-friction, and low-wear performance in current and upcoming applications of MXenes is provided. It is established here that the fundamental understanding of MXenes' mechanical and tribological behavior is essential for their quickly growing applications.Item 2D rare-earth metal carbides (MXenes) Mo2NdC2T2 electronic structure and magnetic properties: A DFT + U study(AIP, 2022) Yao, Shukai; Anasori, Babak; Strachan, Alejandro; Mechanical and Energy Engineering, Purdue School of Engineering and Technology2D rare-earth metal carbides (MXenes) are attractive due to their novel electronic and magnetic properties and their potential as scalable 2D magnets. In this study, we used density functional theory with the Hubbard U correction to characterize the structure, termination, and magnetism in an out-of-plane ordered rare-earth containing M3C2Tx MXene, Mo2NdC2T2 (T = O or OH). We investigated the effect of the U parameter on the stability and magnetism of two possible termination sites: the hollow sites aligned with the inner Nd atoms (Nd-hollow sites) and those aligned with the closest C atoms (C-hollow sites). We found that increasing UMo stabilized the Nd hollow sites, which minimized electrostatic repulsion between C and O atoms. Using UMo = 3.0 eV and UNd = 5.6 eV, obtained via the linear response method, we found that the energetically preferred termination site was C-hollow in Mo2NdC2O2 and Nd-hollow in Mo2NdC2(OH)2. Regardless of termination and the Hubbard U value, we found Mo2NdC2O2 and Mo2NdC2(OH)2 to be magnetic. The C-hollow termination resulted in ferromagnetic states for all Hubbard U tested with no magnetic moment in Mo. In the case of Nd-hollow, Mo became magnetic for UMo ≥ 4 eV. The difference of Mo magnetism in Nd-hollow and C-hollow was explained by crystal field splitting of the Mo d orbital caused by a distorted ligand.Item 2D Titanium Carbide (MXene) Based Films: Expanding the Frontier of Functional Film Materials(Wiley, 2021-11) Li, Guohao; Wyatt, Brian C.; Song, Fei; Yu, Changqiang; Wu, Zhenjun; Xie, Xiuqiang; Anasori, Babak; Zhang, Nan; Mechanical and Energy Engineering, School of Engineering and Technology2D titanium carbide (Ti3C2Tx) MXene films, with their well-defined microstructures and chemical functionality, provide a macroscale use of nano-sized Ti3C2Tx flakes. Ti3C2Tx films have attractive physicochemical properties favorable for device design, such as high electrical conductivity (up to 20 000 S cm–1), impressive volumetric capacitance (1500 F cm–3), strong in-plane mechanical strength (up to 570 MPa), and a high degree of flexibility. Here, the appealing features of Ti3C2Tx-based films enabled by the layer-to-layer arrangement of nanosheets are reviewed. We devote attention to the key strategies for actualizing desirable characteristics in Ti3C2Tx-based functional films, such as high and tunable electrical conductivity, outstanding mechanical properties, enhanced oxidation-resistance and shelf life, hydrophilicity/hydrophobicity, adjustable porosity, and convenient processability. This review further discusses fundamental aspects and advances in the applications of Ti3C2Tx-based films with a focus on illuminating the relationship between the structural features and the resulting performances for target applications. Finally, the challenges and opportunities in terms of future research, development, and applications of Ti3C2Tx-based films are suggested. A comprehensive understanding of these competitive features and challenges shall provide guidelines and inspiration for the further development of Ti3C2Tx-based functional films, and contribute to the advances in MXene technology.Item 2D transition metal carbides (MXenes) in metal and ceramic matrix composites(Springer, 2021-06-02) Wyatt, Brian C.; Nemani, Srinivasa Kartik; Anasori, Babak; Mechanical and Energy Engineering, School of Engineering and TechnologyTwo-dimensional transition metal carbides, nitrides, and carbonitrides (known as MXenes) have evolved as competitive materials and fillers for developing composites and hybrids for applications ranging from catalysis, energy storage, selective ion filtration, electromagnetic wave attenuation, and electronic/piezoelectric behavior. MXenes’ incorporation into metal matrix and ceramic matrix composites is a growing field with significant potential due to their impressive mechanical, electrical, and chemical behavior. With about 50 synthesized MXene compositions, the degree of control over their composition and structure paired with their high-temperature stability is unique in the field of 2D materials. As a result, MXenes offer a new avenue for application driven design of functional and structural composites with tailorable mechanical, electrical, and thermochemical properties. In this article, we review recent developments for use of MXenes in metal and ceramic composites and provide an outlook for future research in this field.Item All-Printed MXene–Graphene Nanosheet-Based Bimodal Sensors for Simultaneous Strain and Temperature Sensing(ACS, 2021-05) Saeidi-Javash, Mortaza; Du, Yipu; Zeng, Minxiang; Wyatt, Brian C.; Zhang, Bowen; Kempf, Nicholas; Anasori, Babak; Zhang, Yanliang; Mechanical Engineering, School of Engineering and TechnologyMultifunctional sensors with integrated multiple sensing capabilities have enormous potential for in situ sensing, structural health monitoring, and wearable applications. However, the fabrication of multimodal sensors typically involves complex processing steps, which limit the choices of materials and device form factors. Here, an aerosol jet printed flexible bimodal sensor is demonstrated by using graphene and Ti3C2Tx MXene nanoinks. The sensor can detect strain by measuring a change in the AC resistive voltage while simultaneously monitoring temperature by detecting the DC Seebeck voltage across the same printed device pattern. The printed bimodal sensor not only expands the sensing capability beyond conventional single-modality sensors but also provides improved spatial resolution utilizing the microscale printed patterns. The printed temperature sensor shows a competitive thermopower output of 53.6 μV/°C with ultrahigh accuracy and stability during both steady-state and transient thermal cycling tests. The printed sensor also demonstrates excellent flexibility with negligible degradations after 1000 bending cycles. The aerosol jet printing and integration of nanomaterials open many opportunities to design and manufacture multifunctional devices for a broad range of applications.Item Beyond Ti3C2Tx: MXenes for Electromagnetic Interference Shielding(ACS, 2020-03) Han, Meikang; Shuck, Christopher Eugene; Rakhmanov, Roman; Parchment, David; Anasori, Babak; Koo, Chong Min; Friedman, Gary; Gogotsi, Yury; Mechanical and Energy Engineering, School of Engineering and TechnologyNew ultrathin and multifunctional electromagnetic interference (EMI) shielding materials are required for protecting electronics against electromagnetic pollution in the fifth-generation networks and Internet of Things era. Micrometer-thin Ti3C2Tx MXene films have shown the best EMI shielding performance among synthetic materials so far. Yet, the effects of elemental composition, layer structure, and transition-metal arrangement on EMI shielding properties of MXenes have not been explored, despite the fact that more than 30 different MXenes have been reported, and many more are possible. Here, we report on a systematic study of EMI shielding properties of 16 different MXenes, which cover single-metal MXenes, ordered double-metal carbide MXenes, and random solid solution MXenes of M and X elements. This is the largest set of MXene compositions ever reported in a comparative study. Films with thicknesses ranging from nanometers to micrometers were produced by spin-casting, spray-coating, and vacuum-assisted filtration. All MXenes achieved effective EMI shielding (>20 dB) in micrometer-thick films. The EMI shielding effectiveness of sprayed Ti3C2Tx film with a thickness of only ∼40 nm reaches 21 dB. Adjustable EMI shielding properties were achieved in solid solution MXenes with different ratios of elements. A transfer matrix model was shown to fit EMI shielding data for highly conductive MXenes but could not describe the behavior of materials with low conductivity. This work shows that many members of the large MXene family can be used for EMI shielding, contributing to designing ultrathin, flexible, and multifunctional EMI shielding films benefiting from specific characteristics of individual MXenes.Item Colloidal Gelation in Liquid Metals Enables Functional Nanocomposites of 2D Metal Carbides (MXenes) and Lightweight Metals(ACS, 2019) Kamysbayev, Vladislav; James, Nicole M.; Filatov, Alexander S.; Srivastava, Vishwas; Anasori, Babak; Jaeger, Heinrich M.; Gogotsi, Yury; Talapin, Dmitri V.; Mechanical Engineering and Energy, School of Engineering and TechnologyNanomaterials dispersed in different media, such as liquids or polymers, generate a variety of functional composites with synergistic properties. In this work, we discuss liquid metals as the nanomaterials’ dispersion media. For example, 2D transition-metal carbides and nitrides (MXenes) can be efficiently dispersed in liquid Ga and lightweight alloys of Al, Mg, and Li. We show that the Lifshitz theory predicts strong van der Waals attraction between nanoscale objects interacting through liquid metals. However, a uniform distribution of MXenes in liquid metals can be achieved through colloidal gelation, where particles form self-supporting networks stable against macroscopic phase segregation. This network acts as a reinforcement boosting mechanical properties of the resulting metal–matrix composite. By choosing Mg–Li alloy as an example of ultralightweight metal matrix and Ti3C2Tx MXene as a nanoscale reinforcement, we apply a liquid metal gelation technique to fabricate functional nanocomposites with an up to 57% increase in the specific yield strength without compromising the matrix alloy’s plasticity. MXenes largely retain their phase and 2D morphology after processing in liquid Mg–Li alloy at 700 °C. The 2D morphology enables formation of a strong semicoherent interface between MXene and metal matrix, manifested by biaxial strain of the MXene lattice inside the metal matrix. This work expands applications for MXenes and shows the potential for developing MXene-reinforced metal matrix composites for structural alloys and other emerging applications with metal–MXene interfaces, such as batteries and supercapacitors.Item Covalent Surface Modification of Ti3C2Tx MXene with Chemically Active Polymeric Ligands Producing Highly Conductive and Ordered Microstructure Films(American Chemical Society (ACS), 2021-11-17) Lee, Jacob T.; Wyatt, Brian C.; Davis, Gregory A., Jr.; Masterson, Adrianna N.; Pagan, Amber L.; Shah, Archit; Anasori, Babak; Sardar, Rajesh; Chemistry, School of ScienceAs interest continues to grow in Ti3C2Tx and other related MXenes, advancement in methods of manipulation of their surface functional groups beyond synthesis-based surface terminations (Tx: −F, −OH, and ═O) can provide mechanisms to enhance solution processability as well as produce improved solid-state device architectures and coatings. Here, we report a chemically important surface modification approach in which “solvent-like” polymers, polyethylene glycol carboxylic acid (PEG6-COOH), are covalently attached onto MXenes via esterification chemistry. Surface modification of Ti3C2Tx with PEG6-COOH with large ligand loading (up to 14% by mass) greatly enhances dispersibility in a wide range of nonpolar organic solvents (e.g., 2.88 mg/mL in chloroform) without oxidation of Ti3C2Tx two-dimensional flakes or changes in the structure ordering. Furthermore, cooperative interactions between polymer chains improve the nanoscale assembly of uniform microstructures of stacked MXene-PEG6 flakes into ordered thin films with excellent electrical conductivity (∼16,200 S·cm–1). Most importantly, our covalent surface modification approach with ω-functionalized PEG6 ligands (ω-PEG6-COOH, where ω: −NH2, −N3, −CH═CH2) allows for control over the degree of functionalization (incorporation of valency) of MXene. We believe that installing valency onto MXenes through short, ion conducting PEG ligands without compromising MXenes’ features such as solution processability, structural stability, and electrical conductivity further enhance MXenes surface chemistry tunability and performance and widens their applications.Item Development Towards Improved Durability Of Implanted Neuroprosthetic Electrodes Through Surface Modifications(2020-08) Vetter, Christian Phillip; Yoshida, Ken; Anasori, Babak; Berbari, EdwardThe present thesis was completed to satisfy two functions in our laboratory: (1) explore carbon-black (CB) as an additive for electrodeposited intrinsically conductive polymers (ICPs) to improve electrical properties across the electrode-electrolyte interface for use in neuromodulation; and (2) design a histology protocol that will analyze peripheral nerve system (PNS) tissue following implantation of conventional metal and modified conventional metal electrodes with the ICP poly(3,4-ethylenedioxythiophere):poly(styrenesulfonate)/carbon-black (PEDOT:PSS/CB). It would appear that the functions explored may seem unrelated, however, these two topics play a crucial role in designing a viable electrode for use in acute and chronic neuromodulation and the subsequent analysis required to determine the mechanical properties and overall biocompatibility of design. A series of experiments with different PEDOT:PSS solutions containing varying amounts of suspended CB (n=19; 0 mg/mL to 2 mg/mL) were explored. Solutions were characterized using cyclic voltammetry (CV) using the intended electrode for deposition, composed of stainless-steel (SS), as the working electrode (WE) to determine respective redox potentials. SS was chosen because of its inherently bad electrochemical properties, meaning that improved functionality post electrodeposition would be easy to identify. Immediately following CV, stainless-steel electrodes were electrodeposited using one of two techniques: (1) potentiostat, allowing the cell to rest at the redox potential required for bipolaron formation (0.9 V); or (2) galvanostat, where the electrode was submitted to a constant current of 200 mA and allowed to coat. Rapid electrochemical impedance spectroscopy was performed prior to and immediately following coating to determine the pre-electrochemical and post-electrochemical impedance characteristics. Results indicate that there was a positive relationship between the amount of CB additive and the relative impedance drop between the uncoated and coated counterparts. Furthermore, the modified electrochemical interfaces are substantially improved for use in frequency ranges of 10 Hz to 50 kHz, which encompass the ranges of our labs recently discovered low frequency alternating current (LFAC) for use in neuromodulation; thus indicating that PEDOT:PSS/CB modification may be used to improve impedance characteristics during our future LFAC experiments. This protocol, the one that contains the ideal concentration of carbon-black, was then recorded and will be used in our lab. Histology protocols were developed to improve our labs capabilities of post-mortem analysis of PNS tissue. Processing and embedding preparations that explored included paraffin, acrylic, and frozen. Subsequently, staining protocols were developed; however, they varied as a function of the embedding media used; staining protocols developed incorporated progressive and regressive hematoxylin and eosin (H&E) staining as well as toluidine blue (TB). Tissue was sectioned and observed using light microscopy.