To advance the MXene field, it is crucial to optimize each step of the synthesis process and create a detailed, systematic guide for synthesizing high‐quality MXene that can be consistently reproduced. In this study, a detailed guide is provided for an optimized synthesis of titanium carbide (Ti3C2T
This content will become publicly available on September 18, 2024
The
- Award ID(s):
- 2409815
- NSF-PAR ID:
- 10492888
- Publisher / Repository:
- RSC Publishing Home
- Date Published:
- Journal Name:
- Materials Advances
- Volume:
- 4
- Issue:
- 18
- ISSN:
- 2633-5409
- Page Range / eLocation ID:
- 4103 to 4109
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
More Like this
-
more » « less
Abstract x ) MXene using a mixture of hydrofluoric and hydrochloric acids for the selective etching of the stoichimetric‐Ti3AlC2MAX phase and delamination of the etched multilayered Ti3C2Tx MXene using lithium chloride at 65 °C for 1 h with argon bubbling. The effect of different synthesis variables is investigated, including the stoichiometry of the mixed powders to synthesize Ti3AlC2, pre‐etch impurity removal conditions, selective etching, storage, and drying of MXene multilayer powder, and the subsequent delamination conditions. The synthesis yield and the MXene film electrical conductivity are used as the two parameters to evaluate the MXene quality. Also the MXenes are characterized with scanning electron microscopy, x‐ray diffraction, atomic force microscopy, and ellipsometry. The Ti3C2Tx film made via the optimized method shows electrical conductivity as high as ≈21,000 S/cm with a synthesis yield of up to 38 %. A detailed protocol is also provided for the Ti3C2Tx MXene synthesis as the supporting information for this study. -
more » « less
Abstract The chemical stability of 2D MXene nanosheets in aqueous dispersions must be maintained to foster their widespread application. MXene nanosheets react with water, which results in the degradation of their 2D structure into oxides and carbon residues. The latter detrimentally restricts the shelf life of MXene dispersions and devices. However, the mechanism of MXene degradation in aqueous environment has yet to be fully understood. In this work, the oxidation kinetics is investigated of Ti3C2T
x and Ti2CTx in aqueous media as a function of initial pH values, ionic strengths, and nanosheet concentrations. The pH value of the dispersion is found to change with time as a result of MXene oxidation. Specifically, MXene oxidation is accelerated in basic media by their reaction with hydroxyl anions. It is also demonstrated that oxidation kinetics are strongly dependent on nanosheet dispersion concentration, in which oxidation is accelerated for lower MXene concentrations. Ionic strength does not strongly affect MXene oxidation. The authors also report that citric acid acts as an effective antioxidant and mitigates the oxidation of both Ti3C2Tx and Ti2CTx MXenes. Reactive molecular dynamic simulations suggest that citric acid associates with the nanosheet edge to hinder the initiation of oxidation. -
more » « less
Abstract Wearable sensors for surface electromyography (EMG) are composed of single‐ to few‐channel large‐area contacts, which exhibit high interfacial impedance and require conductive gels or adhesives to record high‐fidelity signals. These devices are also limited in their ability to record activation across large muscle groups due to poor spatial coverage. To address these challenges, a novel high‐density EMG array is developed based on titanium carbide (Ti3C2T
x ) MXene encapsulated in parylene‐C. Ti3C2Tx is a 2D nanomaterial with excellent electrical, electrochemical, and mechanical properties, which forms colloidally stable aqueous dispersions, enabling safe, scalable solutions‐processing. Leveraging the excellent combination of metallic conductivity, high pseudocapacitance, and ease of processability of Ti3C2Tx MXene, the fabrication of gel‐free, high‐density EMG arrays is demonstrated, which are ≈8 µm thick, feature 16 recording channels, and are highly skin conformable. The impedance of Ti3C2Tx electrodes in contact with human skin is 100–1000× lower than the impedance of commercially available electrodes which require conductive gels to be effective. Furthermore, the arrays can record high‐fidelity, low‐noise EMG, and can resolve muscle activation with improved spatiotemporal resolution and sensitivity compared to conventional gelled electrodes. Overall, the results establish Ti3C2Tx ‐based bioelectronic interfaces as a powerful platform technology for high‐resolution, noninvasive wearable sensing technologies. -
more » « less
Abstract The ability to produce atomically precise, artificial oxide heterostructures allows for the possibility of producing exotic phases and enhanced susceptibilities not found in parent materials. Typical ferroelectric materials either exhibit large saturation polarization away from a phase boundary or large dielectric susceptibility near a phase boundary. Both large ferroelectric polarization and dielectric permittivity are attained wherein fully epitaxial (PbZr0.8Ti0.2O3)
n /(PbZr0.4Ti0.6O3)2n (n = 2, 4, 6, 8, 16 unit cells) superlattices are produced such that the overall film chemistry is at the morphotropic phase boundary, but constitutive layers are not. Long‐ (n ≥ 6) and short‐period (n = 2) superlattices reveal large ferroelectric saturation polarization (P s= 64 µC cm−2) and small dielectric permittivity (εr≈ 400 at 10 kHz). Intermediate‐period (n = 4) superlattices, however, exhibit both large ferroelectric saturation polarization (P s= 64 µC cm−2) and dielectric permittivity (εr= 776 at 10 kHz). First‐order reversal curve analysis reveals the presence of switching distributions for each parent layer and a third, interfacial layer wherein superlattice periodicity modulates the volume fraction of each switching distribution and thus the overall material response. This reveals that deterministic creation of artificial superlattices is an effective pathway for designing materials with enhanced responses to applied bias. -
more » « less
Abstract The oxidation of 2D MXenes jeopardizes their shelf life, both in colloidal dispersions and in functional devices. Certain compounds have been shown to effectively mitigate oxidation of MXenes (such as sodium L‐ascorbate, ascorbic acid, and polyanions), but the nature of interaction between these antioxidants and MXene remains unknown, which impedes the future selection and design of improved protection. This work systematically examines the interactions between three classes of organic antioxidant candidates, α‐hydroxy acids, polycarboxylic acids, and phenols with Ti
n +1Cn Tx MXenes, specifically Ti3C2Tx and Ti2CTx . Interestingly, while some antioxidants provide no protection for the MXenes, and some antioxidants even accelerate their degradation, three antioxidants (e.g., citric acid, tartaric acid, and oxalic acid) protect the MXene nanosheets exceptionally well, showing minimum MXene degradation after the 14‐day storage period. Analysis of the antioxidants’ molecular structure and efficacy suggests that chelation interactions with the transition metal atoms of the nanosheets play a key role in effective protection of MXenes from oxidation.
