Liquid phase exfoliation has evolved to an important and widely used production technique for 2D materials, giving access to large quantities of nanosheets in the liquid phase. Post-exfoliation size selection, for example by liquid cascade centrifugation, can be applied to tune nanosheet lateral sizes and thicknesses. Various starting materials from powders to high-quality crystals can be used for the process. However, the impact of the starting material on the dispersion quality and quantity is widely unexplored. Here, we performed liquid phase exfoliation combined with liquid cascade centrifugation on six different MoS2 starting materials and assessed nanosheet yield, lateral size, and layer number using established quantitative spectroscopic metrics. We show that both yield and nanosheet dimensions are widely unaffected by the choice of the starting material. In contrast, some impact is observed with respect to optical properties, such as photoluminescence of the monolayers. We find that the photoluminescence intensity is lower for small crystallite bulk materials.
Liquid phase exfoliation (LPE) is widely used to produce colloidal dispersions of nanomaterials, in particular two-dimensional nanosheets. The degree of exfoliation, i.e., the length to thickness aspect ratio was shown to be intrinsically limited by the ratio of in-plane to out-of-plane binding strength. In this work, we investigate whether simple pretreatment of the starting material can be used to change the in-plane to out-of-plane binding strength through mild intercalation to improve the sample quality in sonication-assisted LPE. Five different pretreatment conditions of WS2 were tested and the dispersions size-selected through centrifugation. From optical spectroscopy (extinction, Raman, photoluminescence), information on nanosheet dimension (average lateral size, layer number, monolayer size) and optical quality (relative photoluminescence quantum yield) was extracted. We find that the pretreatment has a minor impact on the length/thickness aspect ratio, but that photoluminescence quantum yield can be increased in particular using mild sonication conditions. We attribute this to the successful exfoliation of nanosheets with a lower degree of basal plane defectiveness. This work emphasizes the complexity of the exfoliation process and suggests that the role of defects has to be considered for a comprehensive picture.
Originating from the hexagonal arrangement of magnetic ions in the presence of strong spin orbit coupling, α-RuCl3 is considered as model system for the Kitaev-Heisenberg model. While the magnetic properties of α-RuCl3 have been studied in bulk single crystals or micromechanically-exfoliated nanosheets, little is known about the nanosheets’ properties after exfoliation by techniques suitable for mass production such as liquid phase exfoliation (LPE). Here, we demonstrate sonication-assisted LPE on α-RuCl3 single crystals in an inert atmosphere. Coupled with centrifugation-based size selection techniques, the accessible size- and thickness range is quantified by statistical atomic force microscopy. Individual nanosheets obtained after centrifugation-based size selection are subjected to transmission electron microscopy to confirm their structural integrity after the exfoliation. The results are combined with bulk characterisation methods, including Raman and X-ray photoelectron spectroscopy, and powder diffraction experiments to evaluate the structural integrity of the nanosheets. We report changes of the magnetic properties of the nanomaterial with nanosheet size, as well as photospectroscopic metrics for the material concentration and average layer number. Finally, a quantitative analysis on environmental effects on the nanomaterial integrity is performed based on time and temperature dependent absorbance spectroscopy revealing a relatively slow decay (half-life of ~2,000 h at 20°C), albeit with low activation energies of 6‑20 kJ/mol.
Cardiac magnetic resonance (CMR) examinations require standardization to achieve reproducible results. Therefore, quality control as known as in other industries such as in-vitro diagnostics, could be of essential value. One such method is the statistical detection of long-time drifts of clinically relevant measurements. Starting in 2010, reports from all CMR examinations of a high-volume center were stored in a hospital information system. Quantitative parameters of the left ventricle were analyzed over time with moving averages of different window sizes. Influencing factors on the acquisition and on the downstream analysis were captured. 26,902 patient examinations were exported from the clinical information system. The moving median was compared to predefined tolerance ranges, which revealed an overall of 50 potential quality relevant changes (“alerts”) in SV, EDV and LVM. Potential causes such as change of staff, scanner relocation and software changes were found not to be causal of the alerts. No other influencing factors were identified retrospectively. Statistical quality assurance systems based on moving average control charts may provide an important step towards reliability of quantitative CMR. A prospective evaluation is needed for the effective root cause analysis of quality relevant alerts.
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