Abstract:In order to progress from the lab to commercial applications it will be necessary to develop industrially scalable methods to produce large quantities of defect-free graphene.Here we show that high-shear mixing of graphite in suitable, stabilizing liquids results in large-scale exfoliation to give dispersions of graphene nanosheets. XPS and Raman spectroscopy show the exfoliated flakes to be unoxidised and free of basal plane defects. We have developed a simple model which shows exfoliation to occur once the local shear rate exceeds 10 4 s -1 . By fully characterizing the scaling behaviour of the graphene production rate, we show that exfoliation can be achieved in liquid volumes from 100s of ml up to 100s of litres and beyond. The graphene produced by this method performs well in applications from composites to conductive coatings. This method can be applied to exfoliate BN, MoS2 and a range of other layered crystals. Main Text:Due to its ultra-thin, 2-dimensional nature and its unprecedented combination of physical properties, graphene has become the most studied of all nano-materials. In the next decade graphene is likely to find commercial applications in many areas from high-frequency electronics to smart coatings.
Two-dimensional (2D) transition metal carbides and nitrides (MXenes) have shown outstanding performances in electrochemical energy storage and many other applications. Delamination of MXene flakes in water produces colloidal solutions that are used to manufacture all kinds of products (thin films, coatings, and electrodes, etc.). However, the stability of MXene colloidal solutions, which is of critical importance to their application, remains largely unexplored. Here we report on the degradation of delaminated-Ti3C2T x colloidal solutions (T represents the surface functionalities) and outline protocols to improve their stability. Ti3C2T x MXene solutions in open vials degraded by 42%, 85%, and 100% after 5, 10, and 15 days, respectively, leading to the formation of cloudy-white colloidal solutionss containing primarily anatase (TiO2). On the other hand, the solution could be well-preserved when Ti3C2T x MXene colloidal solutionss were stored in hermetic Ar-filled bottles at 5 °C, because dissolved oxygen, the main oxidant of the MXene flakes, was eliminated. Under such a recipe, the time constant of the solution was dramatically increased. We have found that the degradation starts at the edges and its kinetics follows the single-exponential decay quite well. Moreover, we performed size selection of the MXene solution via a cascade technique and showed that the degradation process is also size-dependent, with the small flakes being the least stable. Furthermore, a dependence between the degradation time constants and the flake size allows us to determine the size of the nanosheets in situ from UV–vis spectra and vice versa. Finally, the proposed method of storing the MXene colloidal solution in Ar-filled vials was applied to Ti2CT x to improve its stability and time constant, demonstrating the validity of this protocol in improving the lifetime of different MXene solutions.
Transition metal dichalcogenides have a laminar structure, with strongly covalently bonded layers weakly interacting through van der Waals forces. They are of special interest also because of their unique properties once exfoliated in nanoflakes. We analyse the microstructure of oxidised TiS 2 nanoflakes with atomically resolved scanning transmission electron microscopy and propose a comprehensive model for their reactivity by means of first principles simulations. In particular we find that reaction to water proceeds from the edges of the flake, while it is thermodynamically possible but kinetically hindered in the middle, unless it is initiated by the presence of a surface vacancy. Importantly O substitution for S allows fine-tuning control of the flake bandgap, paving the way for the use of TiS 2-x O x alloys as surface catalysts and photovoltaic materials. . High-resolution image of a TiS 2 flake edge showing an extended crystalline region in the upper part. The bright dots in the image correspond to Ti atoms surrounded by S atoms. Below the dotted line an area of amorphous TiO2 is indicated. In the magnified HAADF image (blue box in the image) the Ti and S atom columns are well separated. Beside the HAADF image we present the corresponding Electron Energy Loss (EEL) spectrum images (elemental maps) of S, C, Ti and O respectively (left to right) for the same region. These elemental maps confirm that the bright areas in the HAADF STEM image are indeed Ti atoms, surrounded by S. In the part of the The O signal is predominantly localised at the edge (dotted region). Some C contamination can be seen, especially at the edge. b) FFT of Survey image in (a) (gamma set to 0.4 to suppress the background) and c) the EELS sum-spectrum used to produce the elemental maps presented in (a). The low signal to background ratio at the O edge explains the noise in the O-map..
E -m a i l : b e a t r i x . m e n d o z a @ g m a i l . c o m"These authors contributed equally to this work Abstract Manganese oxide nanosheets were synthesized using liquid-phase exfoliation that achieved suspensions in isopropanol with concentrations of up to 0.45 mg ml -1 . A study of solubility parameters showed that the exfoliation was optimum in N,N-Dimethylformamide followed by isopropanol and diethylene glycol. Isopropanol was the solvent of choice due to its environmentally friendly nature and ease of use for further processing. For the first time, a hybrid of graphene and manganese oxide nanosheets was synthesized using a single-step co-exfoliation process. The 2D hybrid was synthesized in isopropanol suspensions with concentrations of up to 0.5 mg ml -1 and demonstrated stability against re-aggregation for up to 6 months. The co-exfoliation was found to be a energetically favorable process in which both solutes, graphene and manganese oxide nanosheets, exfoliate with an improved yield as compared to the single-solute exfoliation procedure. This work demonstrates the remarkable versatility of liquid-phase exfoliation *To whom correspondence should be addressed 2 with respect to the synthesis of hybrids with tailored properties, and it provides proof-of-concept ground work for further future investigation and exploitation of hybrids made of two or more 2D nanomaterials that have key complementary properties for various technological applications.
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