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Abstract Structural color arises from light scattering rather than organic pigments and can be found in Nature, such as in bird feathers and butterfly wings. Synthetic materials can mimic Nature by leveraging materials with contrasting optical characteristics by controlling each materials’ spatial arrangement in a heterostructure. Two-dimensional MXene nanosheets are particularly interesting due to their unique optical properties, but MXenes have not been used directly as a structural colorant because it is challenging to control the spatial placement of MXenes at the nanometer level. Here, we report the emergence of structural color in layer-by-layer (LbL) assemblies of Ti₃C₂T_zMXene nanosheets and polyelectrolyte heterostructures with controlled block thicknesses. The block thickness and spatial placement of MXene are controlled by the assembly’s salt concentration and number of layer pairs. This work demonstrates that optical characteristics of MXene/polyelectrolyte heterostructures depend on MXene content and placement, while deepening the understanding of MXenes within structural color films. 

Rapid, out‐of‐oven techniques for MXene synthesis are of great interest and would allow for easier production of this exciting class of 2D materials. MXenes are typically synthesized by etching MAX phases with strong acids for long times, sometimes exceeding 40 h. Electrothermal synthesis techniques can reduce the heating time of materials; here Joule heating with molten salt etching precursors is utilized to etch MAX phase into multilayered (ML) Ti₃C₂T_x MXenes. An inert environment is used to etch the MAX phase in 30 min at 750–800 °C. SEM/EDS and XRD confirmed etching of the material. XPS, FTIR, and Raman are compared to conventional LiF‐HCl ML‐ Ti₃C₂T_x, showing similar spectra to Joule heated ML‐Ti3C2Tx material. Most importantly, this new out‐of‐oven Ti₃C₂T_x synthesis decreased etching time by 98% from molten salt etching and reduced energy usage from 1.56 × 10⁷to 1.01 × 10⁶J g⁻¹per batch, paving the way for the commercialization of MXene etching. 

Industrial scaleup of MXene synthesis has faced many challenges, both in the process safety and nanosheet yield. As a step toward the scalability of MXenes, we carried out a one-to-one comparison of the industrial scalability and application performance of two methods for producing Ti3C2Tz MXenes: LiF-HCl acid etching and Lewis acid molten salt etching. This study had an emphasis on nanoscale structure, electrical conductivity, electromagnetic interference (EMI) shielding and supercapacitive properties, yield, and process scalability, both at the etched clay stage and delaminated nanosheet stage. This comparison was completed in parallel with the same starting MAX phase, chemicals, and processing equipment, where necessary. The synthesis process influences the structure and terminal groups of MXenes, altering properties and performance. Notably, the electrical conductivity was superior for acid-etched nanosheets at 2200 S/cm, compared to salt-etched nanosheets at 0.66 S/cm. For EMI shielding effectiveness and capacitance, acid-etched nanosheets performed the highest. The yield of the acid-etched nanosheets was ~ 50% and salt-etched nanosheets was 15%. The acid-etched process was scaled up with a small business partner from 1-g to 200-g MAX phase, with similar properties and yield. When the salt-etching process was scaled up to 25 g of MAX, the properties remained similar to the 1 g batch, with a lower yield of ~ 5%. Although the acid-etching process was better for most metrics, the molten salt-etching method is still in its infancy and has advantages regarding process safety. 

Not AvailableIntercalation in two-dimensional (2D) materials can modify their physical, chemical, and electronic properties. This modification enables the tailoring of 2D material characteristics, enhancing their performance and expanding their applications in various fields. The friction performance of 2D materials such as MoS2 and graphite has a strong dependence on their interlayer spacing, and they exhibit an increase in d-spacing associated with a reduction in friction performance. The ability to control the interlayer spacing of Ti3C2Tz MXene has proven beneficial for energy storage applications such as batteries and supercapacitors, but no one has utilized this control of interlayer spacing for lubrication. In this study, we demonstrate that interlayer spacing of multilayer (ML) Ti3C2Tz MXene can be controlled through chemical intercalation and its direct effects on the electrical conductivity and friction performance. We observed a notable decrease in electrical conductivity in vacuum-filtered ML-Ti3C2Tz MXene films, which was attributed to an increased internal resistance resulting from the expansion of the interlayer gap. We also found a significant reduction in the coefficient of friction for ML-Ti3C2Tz MXene with an increased d-spacing. This reduction is attributed to a weakened attraction of individual ML-Ti3C2Tz MXene layers (intercalated). Under a tangential force, it becomes easier to slide within the larger interlayer gap with weakened van der Waals forces. This work provides insights into the tunability of MXene properties through interlayer spacing, offering potential applications requiring materials with specific electrical and friction characteristics. 

The major challenge to fabricate MXene/polymer composites are the processing conditions and poor control over the distribution of the MXene nanosheets within the polymer matrix. Traditional ways involve the direct mix of fillers and polymers to form a random homogeneous composite, which leads to inefficient use of fillers. To address these challenges, researchers have focused on the development of ordered MXene/polymer composite structures using various fabrication strategies. In this review, we summarize recent advances of structured MXene/polymer composites and their processing-structure-property relationships. Two main forms of MXene/polymer composites (films and foams) are separately discussed with a focus on the detailed fabrication means and corresponding structures. These architected composites complement those in which MXenes nanosheets are isotropically dispersed throughout, such as those formed by aqueous solution mixing approaches. This review culminates in a perspective on the future opportunities for architected MXene/polymer composites. 

Although surface terminations (such as ═O, –Cl, –F, and –OH) on MXene nanosheets strongly influence their functional properties, synthesis of MXenes with desired types and distribution of those terminations is still challenging. Here, it is demonstrated that thermal annealing helps in removing much of the terminal groups of molten salt-etched multilayered (ML) Ti3C2Tz. In this study, the chloride terminations of molten salt-etched ML-Ti3C2Tz were removed via thermal annealing at increased temperatures under an inert (argon) atmosphere. This thermal annealing created some bare sites available for further functionalization of Ti3C2Tz. XRD, EDS, and XPS measurements confirm the removal of much of the terminal groups of ML-Ti3C2Tz. Here, the annealed ML-Ti3C2Tz was refunctionalized by −OH groups and 3-aminopropyl triethoxysilane (APTES), which was confirmed by FTIR. The −OH and APTES surface-modified ML-Ti3C2Tz are evaluated as a solid lubricant, exhibiting ∼70.1 and 66.7% reduction in friction compared to a steel substrate, respectively. This enhanced performance is attributed to the improved interaction or adhesion of functionalized ML-Ti3C2Tz with the substrate material. This approach allows for the effective surface modification of MXenes and control of their functional properties.