Mild Sonication Research Articles

Electrochemical Lithium Intercalation & Exfoliation in 2D TMDs and Its in-Situ Studies

We developed a lithium ion battery intercalation & exfoliation method with detailed experimental procedures for the mass production of 11 two dimensional TMDs and inorganic nanosheets, such as MoS2, WS2, TiS2, TaS2, ZrS2, graphene, h-BN, NbSe2, WSe2, Sb2Se3 and Bi2Te3, among them 3 TMDs achieved mono- or double layer yield > 90%. This method involves the electrochemical intercalation of lithium ions into layered inorganic materials and a mild sonication process. The Li insertion can be monitored and finely controlled in the battery testing system, so that the galvanostatic discharge process is stopped at a proper Li content to avoid decomposition of the intercalated compounds. The intercalation strategy can also be used to tune 2D TMDs’ physical and chemical properties for various applications. For example, we developed a one-step covalent functionalization method on MoS2 nanosheets for membrane fabrication, which exhibited excellent water desalination performance. For lithium intercalation mechanism, the state-of-the-art In-Situ Liquid Phase TEM is an ideal technique for identifying the phase changes during intercalation process. With self-designed electrochemical liquid cell utilized, we can directly vapture the dynamic electrochemical lithiation and delithiation of electrode in a commercial LiPF6/EC/DEC electrolyte, such as LiF nanocrystal formation, lithium metal dendritic growth, electrolyte decomposition, and solid-electrolyte interface (SEI) formation. Combining with other in-situ techniques, such as in-situ XAS, XRD and Raman, etc, the underlying lithium intercalation mechanism in TMDs were further investigated, which render us a comprehensive understanding of the intrinsic correlation between the intercalation process and TMDs.

Contact‐Engineering of Self‐Aligned‐Gate Metal Oxide Transistors Processed via Electrode Self‐Delamination and Rapid Photonic Curing

AbstractMetal oxide thin‐film transistors (TFTs) offer remarkable opportunities for applications in emerging transparent and flexible microelectronics. Unfortunately, their performance is hindered by limitations associated with parasitic effects, such as parasitic electrode overlap capacitances and high contact resistance, which can severely limit their dynamic behavior. Here, an innovative method is reported to fabricate coplanar self‐aligned‐gate (SAG) indium‐gallium‐zinc‐oxide (IGZO) transistors with engineered source/drain contacts. The manufacturing process starts with the deposition and patterning of a gate electrode/dielectric stack and its functionalization with an organic self‐assembled monolayer (SAM) as the surface energy modifier. A second gold (Au) electrode is subsequently deposited over the gate electrode stack. The overlapping region between the two electrodes is removed via self‐delamination under mild sonication, forming perfectly aligned coplanar Au‐Gate‐Au electrodes. Device fabrication is completed with the spin coating of the IGZO precursor, followed by rapid photonic curing. Replacing the gold source/drain contact with bimetallic electrodes such as Au/In and Au/ITO enables a reduction in contact resistance and improves the transistor performance remarkably without increasing manufacturing complexity. The method is highly scalable, robust, and applicable to other semiconductor materials.

Swellable hybrid silicas for the removal of rhodamine B dye from aqueous phase

This study is focused on the use of a hybrid organic-inorganic silica (Silica-SOM) for the removal of Rhodamine B dye (RhB) from water media. Because of its hybrid structure, Silica-SOM has the unique property of being swellable in the presence of an organic solvent, thus increasing the volume available for pollutants adsorption. The adsorption capacity of the Silica-SOM to adsorb RhB from water media has been determined. In particular, if the material is previously swollen with an organic solvent, it is able to sequester more than 99 % of dye molecules in a 1.0 × 10−5 M RhB solution in less than 1 h at ambient conditions. In addition, the ability of Silica-SOM to be re-generated by mild sonication in ethanol after one RhB adsorption cycle was tested for the first time: the material was easily regenerated and used for six consecutive adsorption cycles; in each of them there is no loss in adsorption performance, which remains quantitatively high and extremely fast.

Electron beam-assisted exfoliation of boron nitride and covalent functionalization

A facile, scalable exfoliation technique is still required for further modification to cater to any potential application for two-dimensional boron nitride. This paper discusses the radiation-assisted exfoliation of hexagonal boron nitride (h-BN) using electron beam irradiation and followed by functionalization with phosphoric acid 2-hydroxyethyl methacrylate ester (PA) to facilitate targeted applications. h-BN is dispersed in NaOH solution and subjected to mild sonication to facilitate ion intercalation between the layers. The sonicated h-BN solution was exposed to electron beam irradiation for BNNS exfoliation. The degree of exfoliation was measured in terms of d-spacing derived from XRD using Bragg's law. The effect of irradiation dose, energy, NaOH concentration, and mass of h-BN, on exfoliation degree was investigated. XRD analysis was used to compute the d-spacing, crystallinity, and crystal size of h-BN after irradiation. The d-spacing attained for pristine h- BN was 0.334 nm, however it increases to 0.337 nm upon irradiation at 100 kGy doses, 3 MeV of energy, and 0.1 g of h-BN in 80 mL of 30 % NaOH solution. The occurrence of radiation-assisted exfoliation and its mechanism were supported by FTIR, TGA, Raman, FESEM, XPS, AFM, and TEM analyses. The exfoliated BN was functionalized with PA. The degree of functionalization was measured by phosphoric density (mmol/g) via the acid-base titration method. The effect of PA concentration, reaction temperature and mass on phosphoric density was also investigated. The highest phosphoric density attained was approximately 13.32 mmol/g at 10 % PA, 0.1 g of exfoliated BN, 80 °C, and 5 h. The incorporation of PA onto exfoliated BN was further confirmed by XRD, FTIR, TGA, Raman, FESEM-EDX, and XPS analyses. Conclusively, this study reveals a facile dual-step exfoliation and functionalization technique of h-BN nanosheet through radiation assisted exfoliation technique.

Synergistic effect on dispersion, thermal conductivity and mechanical performance of pyrene modified boron nitride nanotubes with Al2O3/epoxy composites

Due to the intrinsic attributes of boron nitride nanotubes (BNNT), its assimilation into composite materials displays an immense potential for thermal performance augmentation. However, the presence of Van der Waals forces and hydrophobicity of BNNT causing interfacial incompatibility with the polymeric matrix greatly hinders its practical applications. This instigates a dispersion dilemma and subsequent agglomeration of BNNT in the polymer matrix, which massively hampers the thermal performance of the polymer composites. In this respect, we here present a facile BNNT modification strategy; deposition of amine-attached pyrene (PAA) on the BNNT surface through a mild sonication process. The presence of amine in the pyrene molecules reduces the surface tension of PAA deposited BNNT (BNNT-PAA) allowing it to be readily dispersed in the various solvents even at the high concentrations. BNNT-PAA was added as a co-filler along with a primary filler (Al2O3) in the epoxy resin. The formed epoxy composites presented an improvement of as much as 33.1 % in tensile strain and 175.8 % in tensile stress with the addition of 1wt% of BNNT-PAA, while the thermal conductivity of vertical direction was enhanced as high as 62.3 %, possibly due to the constructed BNNT thermal conducting channels among alumina particles.

Preparation of a ruthenium complex covalently bonded to multilayer graphene and its evaluation as a photocatalyst.

Multilayer graphene (MLG), obtained by mild sonication of graphite in NMP, was functionalised via 1,3-dipolar cycloaddition with azomethine ylides generated by thermal 1,2-prototropy from various imino esters. The microwave-assisted functionalisation took place in five hours at 100 °C. The resulting MLG, containing substituted proline-based amine functional groups, was characterized using XPS and showed a nitrogen loading three times that obtained for the same transformation performed for five days using convection-assisted heating. The preparation of the imino ester containing a bipyridine unit at the arylidene position allowed for the preparation of the corresponding functionalised MLG, which incorporated the ruthenium atom to achieve a heterogeneous MLG-Ru complex. This supported complex was tested, as a proof of concept, as a photocatalyst of the aerobic oxidative hydroxylation of 4-methoxyphenylboronic acid.

Impact of ultrasound treatment on the physicochemical and rheological properties of acid hydrolyzed sorghum starch

The present study aimed to evaluate the influence of ultrasonication on the physicochemical properties of native and acid-hydrolyzed white sorghum starch. Sorghum starch exhibited improved freeze-thaw stability, solubility, swelling power, and paste clarity after mild sonication. Starches sonicated at 30 % amplitude for 10 and 20 min increased the peak viscosity to 249 and 240 BU, gel firmness to 140.23 and 131.62 (g), ΔH to 13.4 and 13.1 (J/g), crystallinity to 29.51 and 29.10 (%), double helix content to 1.11 and 1.07 and degree of ordered structures to 1.16 and 1.09. The sonicated dual-treated samples (sonicated-acid hydrolyzed) exhibited reduced swelling power, peak viscosity, gelatinization temperatures and gel firmness. In contrast, the solubility, paste clarity, ΔH, percentage of crystallinity, double helix content and degree of ordered structures improved. Ultrasonic treatment made cracks and holes in the granule surface, whereas dual-treated starches were more porous and rougher, with deep depressions. All sorghum starches displayed shear-thinning behavior (n < 1). The pseudoplastic behavior and consistency indices of the starch paste decreased with increasing sonication time and amplitude. The G' was always higher than G" and tanδ was <1 for all samples, indicating a more solid/elastic behavior. The increased sonication time and amplitude, as well as the dual-treatment, caused the gel to become more susceptible to shear forces, which resulted in a decrease in G' and G" and an increase in tanδ.

Human Nanoplatelets as Living Vehicles for Tumor-Targeted Endocytosis In Vitro and Imaging In Vivo

Recent studies have shown human platelets can access the tumor microenvironment by passive diffusion across capillaries or via activated immune cells. In a previous study, we exploited this affinity of platelets for tumor cells as part of a new approach to target tumors with modified platelets. Therefore, the engineering of human nanoplatelets as living vehicles for in vivo tumor-targeted near-infra-red fluorescence (NIRF) imaging and the delivery of cytotoxins to tumor cells by endocytosis are described in this study. Nanoplatelets with an average diameter of 200 nm were prepared by mild sonication of kabiramide C (KabC)-loaded human platelets. The sealed plasma membrane of the nanoplatelets allows them to accumulate and retain membrane-permeable chemicals, such as epidoxorubicin (EPI) and KabC. Tumor-targeted imaging functionalities were engineered on the nanoplatelets by surface-coupling transferrin, Cy5 and Cy7. High-resolution fluorescence imaging and flow cytometry analyses showed that the nanoplatelets loaded with EPI and Cy5 targeted human myeloma cells (RPMI8226 cells) that over-expressed the transferrin receptor. The endocytosis of the nanoplatelets by RPMI8226 cells was transferrin-dependent and induced apoptosis. The test results also showed that the nanoplatelets functionalized with transferrin and Cy7 and injected in mice bearing RPMI8226 cells-derived myeloma xenotransplants accumulated in the tumor tissue and could be used for high-contrast in vivo NIRF imaging of early-stage tumors. Nanoplatelets represent a new class of living nano-vehicles that may efficiently target and deliver therapeutic agents and imaging probes to diseased tissues including tumors.

Green synthesis of ultrathin 2D nanoplatelets, hematene and magnetene, from mineral ores in water, with strong optical limiting performance

Hematene and magnetene nanoplatelets have been produced by liquid phase exfoliation of natural mineral ores, in a water solution of melamine under mild sonication.

Augmentation in polyhydroxybutyrate and biogas production from waste activated sludge through mild sonication induced thermo-fenton disintegration

In this study, an innovative approach was developed to enhance the hydrolysis through phase-separated pretreatment by removing exopolymeric substances via mild sonication followed by thermo-Fenton disintegration. The exopolymeric substances fragmentation was enhanced at the sonic specific energy input of 2.58 kJ/kg total solids. After exopolymeric substance removal, the disintegration of biomass by thermo-Fenton yield the solubilization of 29.8 % at Fe2+:H2O2 dosage and temperature of 0.009:0.036 g/g suspended solids and 80 °C as compared to thermo-Fenton alone disintegration. The polyhydroxybutyrate content of 93.1 % was accumulated by Bacillus aryabhattai at the optimum time of 42 h, while providing 70 % (v/v) pre-treated supernatant as a carbon source under nutrient-limiting condition. Moreover, the biogas generation of 0.187 L/g chemical oxygen demand was achieved using settled pretreated sludge. The pretreated sludge sample thus served as a carbon source for polyhydroxybutyrate producers as well as substrate for biogas production.

Effective control of antibiotic resistance using a sonication-based combinational treatment and its application to fresh food

Antibiotics have been widely used to treat several infectious diseases. However, the overuse of antibiotics has promoted the emergence and spread of antibiotic resistant bacteria (ARB) in various fields, including the food industry. In this study, the antimicrobial efficacies of two conventional sterilization methods, mild heat, and sonication, were evaluated and optimized to develop a new strategy against ARB. Simultaneous mild heat and sonication (HS) treatment led to a significant reduction in viable cell counts, achieving a 5.58-log reduction in 4 min. However, no remarkable decrease in viable cell counts was observed in individually treated groups. Interestingly, the release of antibiotic resistance genes (ARGs) increased in a time-dependent manner in the heat-treated and HS-treated groups. The inactivation levels of ARGs increased as the HS treatment time increased from 2 to 8 min, and most ARGs were degraded after 8 min. In contrast, no significant inactivation of ARGs was observed in the heat-treated and sonication-treated groups after 8 min. These results reveal the synergistic effect of the combination treatment in controlling not only ARB but also ARGs. Finally, on applying this newly developed combination treatment to fresh food (cherry tomato and carrot juice), 3.97- and 4.28-log microbial inactivation was achieved, respectively. In addition, combination treatment did not affect food quality during storage for 5 days. Moreover, HS treatment effectively inactivated ARGs in fresh food systems.

Effect of ultrasound on the glycosylation reaction of pea protein isolate–arabinose: Structure and emulsifying properties

This study investigated the effects of different ultrasonic power and ultrasonic time on the structure and emulsifying properties of pea protein isolate (PPI)–arabinose conjugates. An examination of the absorbance and color development of PPI-d-arabinose (Ara) conjugates found that compared with traditional heating, the degree of glycosylation of protein reached the maximum when the ultrasonic treatment power was 150 and the treatment time was 30 min. Structural analysis revealed that the content of disordered structures (β-turn and random coil) of the protein conjugates increased, the maximum emission wavelength of the fluorescence spectrum was red-shifted, and the UV second-order derivative values decreased. The protein structure unfolded, exposing more hydrophobic groups on the molecular surface. Ultrasonic treatment improved the emulsification of protein conjugates. The emulsifying activity index (EAI) increased to 19.7 and 19.3 m2/g, and the emulsifying stability index (ESI) also increased. The contact angle and zeta potential also demonstrate that ultrasonic power has a positive effect on emulsion stability. Based on examining the thermal stability of the emulsion, the ultrasonic treatment increased the thermal denaturation resistance of the protein. This result confirms that mild sonication can increase the degree of glycosylation reaction and improve the emulsification properties of protein–Ara conjugates, providing a theoretical basis for developing foods with excellent emulsification properties.

Skin-targeted delivery of extracellular vesicle-encapsulated curcumin using dissolvable microneedle arrays

Therapeutic benefits of curcumin for inflammatory diseases have been demonstrated. However, curcumin's potential as a clinical therapeutic has been hindered due to its low solubility and stability in vivo. We hypothesized that a hybrid curcumin carrier that incorporates albumin-binding and extracellular vesicle (EV) encapsulation could effectively address the current challenges of curcumin delivery. We further postulated that using dissolvable microneedle arrays (dMNAs) for local delivery of curcumin-albumin-EVs (CA-EVs) could effectively control skin inflammation in vivo. Mild sonication was used to encapsulate curcumin and albumin into EVs, and the resulting CA-EVs were integrated into tip-loaded dMNAs. In vitro and in vivo studies were performed to assess the stability, cellular uptake, and anti-inflammatory bioactivity of dMNA-delivered CA-EVs. Curcumin in CA-EVs exhibited at least five-fold higher stability in vitro than naïve curcumin or curcumin-EVs without albumin. Incorporating CA-EVs into dMNAs did not alter their cellular uptake or anti-inflammatory bioactivity. The dMNA embedded CA-EVs retained their bioactivity when stored at room temperature for at least 12 months. In rat and mice models, dMNA delivered CA-EVs suppressed and significantly reduced lipopolysaccharide and Imiquimod-triggered inflammation. We conclude that dMNA delivery of CA-EVs has the potential to become an effective local-delivery strategy for inflammatory skin diseases. Statement of significanceWe introduce and evaluate a skin-targeted delivery system for curcumin that synergistically combines albumin association, extracellular-vesicle encapsulation, and dissolvable microneedle arrays (dMNAs) . In vitro, curcumin-albumin encapsulated extracellular vesicles (CA-EVs) inhibit and reverse the LPS-triggered expression of inflammatory transcription factor NF-κB. The integration of CA-EVs into dMNAs does not affect them physically or functionally. Importantly, dMNAs extend EV storage stability for at least 12 months at room temperature with minimal loss in their bioactivity. We demonstrate that dMNA delivered CA-EVs effectively block and reverse skin inflammation in vivo in mouse and rat models.

Degree of oxidation of sonicated soybean oil using various sonication process parameters

SummaryThis research aimed to examine the effect of high‐intensity ultrasound (HIU) on the oxidation of soybean oil (SBO). Samples (5, 100, and 250 g) were sonicated at 25 °C using various sonication conditions: power level (settings 1, 5, and 9), tip size (12.7, 3.2, and 2 mm), and duration (5, 10, and 60 s). After sonication, the degree of oxidation of samples (sonicated and non‐sonicated SBO) were analysed using peroxide value (PV), oil stability index (OSI), and volatile compounds. Sonication was applied to obtain a range of absolute power (0–123.5 W), power density (0–14.2 W cm−3), and power intensity (0–1,120 W cm−2) values. The highest power density and power intensity were obtained with the highest HIU setting with the 3.2 mm tip. The highest power was obtained when HIU was applied using a 12.7 mm tip and setting 9 in 250 g of sample. No significant difference (P &gt; 0.05) was observed in PV (0.20 ± 0.01 mEq kg−1) nor OSI (10.05 ± 0.04 h), among the various sonication conditions tested. In addition, no differences were observed in the volatile compounds obtained. These results show that HIU can be used under mild sonication conditions such as the ones needed to change the physical properties of lipids without causing oxidative deterioration.

Facile Edge Functionalization of Graphene Layers with a Biosourced 2-Pyrone

Edge functionalization of graphene layers is of great interest in the field of materials chemistry: the properties of graphene are substantially unaltered and its compatibility and chemical reactivity with various environments can be tuned. In this work, edge functionalization of graphene layers was performed with a 2-pyrone, ethyl 3-hydroxy-2-oxo-2H-pyran-6-carboxylate (Pyr-COOEt). 2-Pyrones are C-6 unsaturated heterocyclic sugar derivatives and are intriguing building blocks for the preparation of innovative chemical structures. Sodium 3-acetoxy-2-oxo-2H-pyran-6-carboxylate was prepared starting from mucic acid, in a one-pot synthesis with a yield of about 74%, and was then transformed into the acid and then into ethyl ester derivatives. The adduct of Pyr-COOEt with a high surface area graphite (HSAG) was obtained by simply mixing and donating energy, either thermal or mechanical. The functionalization yield was estimated from thermogravimetric analysis (TGA) data and was found to be up to 91%. The adducts were characterized by Fourier transform infrared and Raman spectroscopies and wide-angle X-ray diffraction. The presence of pyrone in the adduct was clearly detected in the IR spectra, and the bulk structure of the graphitic substrate was found to be substantially unaltered by the functionalization reaction. The experimental findings suggest that the edge functionalization of the graphene layers occurred. Stable water dispersions of HSAG/Pyr adducts were prepared and studied through ultraviolet–visible analysis. Aggregates of few-layer graphene were obtained by mild sonication and centrifugation, as revealed by high-resolution transmission electron microscopy. This paper shows that a biobased molecule can be used for selectively decorating the edges of graphene layers, with oxygenated functional groups having a defined chemical structure and avoiding the use of oil-based, dangerous, and even noxious ingredients. The most plausible interpretation for the formation of the HSAG adduct with 2-pyrone seems to be the cycloaddition reaction between the edges of the graphitic substrate and the unsaturated biomolecule. Such a functionalization appears to be suitable for a scale up and paves the way for the preparation of a variety of derivatives.

Power ultrasound to enhance the fermentation process of traditional Taiwanese rice wine

AbstractRice wine is a fermented product that can be distilled to produce rice spirit, which is an ingredient in several Asian dishes. The industry usually uses traditional practices for rice wine production. This study aims to evaluate the possibility of enhancing Taiwanese rice wine fermentation through the application of ultrasound as an emerging technology. In this regard, in an academic‐industrial cooperation, a commercial process was modified by incorporating a 550‐W power horn ultrasound treatment after the saccharification step. Independent parameters were sonication times of 0, 3, 6, 9, and 12 min (referred to as control, US3, US6, US9, and US12, respectively) and fermentation time (0, 2, 4, 6, qnd 8 days), and dependent parameters were total phenolic content (TPC), total acidity, alcohol content, CIE color values, pH, total acidity, electrical conductivity (EC), and refractive index (RI). The results showed that US3 provided the highest alcohol content while the physical characteristics, including pH, total acidity, EC, and RI, were not significantly different from those of the control sample. At the same time, sonication alters color values (L*, a*, b*, color intensity, and overall color changes) and TPC. Besides, US12 treatment yielded a rice wine with the highest TPC, that is, 306.77 ± 1.90 mg GAE/L sample. Therefore, sonication conditions can be optimized to achieve the desired properties such as the highest alcohol content or highest TPC. This study revealed that a relatively mild sonication process can enhance the fermentation process to achieve higher alcohol content which could be related to the stress‐response of yeast (Saccharomyces cerevisiae) and modification of fermentation medium. This can be considered an effort to contribute to sustainable development goals (SDGs) and sustainability by increasing resource efficiency. Besides, a more intense sonication resulted in a fermented product with higher amounts of bioactive compounds through the improved extraction process. According to the observations, power ultrasound is a promising pretreatment to boost the fermentation process and rice wine quality through positive effects on both brewer's yeast and fermentation substrates.Practical ApplicationsThe wine processing industry is seeking innovative approaches to enhance the fermentation yield, reduce fermentation time, and enhance the production capacity. In this sense, the results of this industrial‐academic collaborative research showed that power ultrasound has the potential to improve rice wine fermentation to meet the above‐mentioned industrial demands. This emerging technology at appropriate processing conditions enhanced the percentage of alcohol in the final product which could be considered as an approach to enhance the profit of wineries through enhancing the resource efficiency, that is, more amount of product from the same amount of raw materials. At the same time, this sonication‐based technique did not negatively affect the physicochemical properties of the rice wine. The production platform explored in this study is scalable and can be implemented at industrial levels in wineries.

Bridge between mass transfer behavior and properties of bubbles under two-stage ultrasound-assisted physisorption of polyphenols using macroporous resin

Ultrasound is efficient to enhance various mass transfer processes. This study demonstrates that both ultrasound pretreatment and ultrasonication during adsorption promote the physisorption of polyphenols. The time to reach the adsorption equilibrium was shortened by more than 90 % when the resin diameter deceased from 592 μm to 60.23 μm in the intensive ultrasound pretreatment. The mass transfer mechanism of adsorption under mild sonication differs from that of adoption with intensive ultrasound pretreatment. Mild sonication during adsorption strengthens the influence of surface diffusion of polyphenols on intraparticle diffusion. In contrast, severe disruption of resin particles due to intensive ultrasound pretreatment weakens the surface diffusivity of polyphenols and reduces the contribution of surface diffusion. Also, the physics and sonochemistry of cavitation under sonication environments were explored. Under intensive and mild ultrasound treatments, the calculated bubble numbers were approximately 18789 L-1 and 6312 L-1, respectively. Moreover, a relationship was established between adsorption capacity from mass transfer modeling and bubble properties including the bubble collapse pressure, bubble number, processing time, and processing scale. This bridge between mass transfer behavior and properties of bubbles provides guidance and new insight for the design and scale-up of the ultrasound-assisted adsorption.

F-diamane-like nanosheets from expanded fluorinated graphite

Ultrathin diamond (diamane)-like films or nanosheets have recently been experimentally obtained through chemically induced phase transition (e.g., fluorination) of bilayer graphene films or graphite flakes. To fully exploit the properties of diamane, further advances in the synthesis methods for its large-scale production are required. Herein, we report a new route for the efficient and high-yield production of fluorinated diamane (F-diamane)-like nanosheets. This is achieved by direct fluorination of expandable graphite or thermally expanded graphite with molecular fluorine to form stage-2 graphite fluoride (C2F)n made of stacked layers of F-diamane. Subsequently, mild sonication is implemented to exfoliate the layers into F-diamane-like nanosheets of hundreds of nanometers to a few micrometers in lateral size, with a thickness of mostly < 10 nm.

High-yield production of mono- or few-layer transition metal dichalcogenide nanosheets by an electrochemical lithium ion intercalation-based exfoliation method.

Transition metal dichalcogenide (TMD) nanomaterials, especially the mono- or few-layer ones, have received extensive research interest owing to their versatile properties, ranging from true metals (e.g., NbS2 and VSe2) and semimetals (e.g., WTe2 and TiSe2) to semiconductors (e.g., MoS2 and We2) and insulators (e.g., HfS2). Therefore, the reliable production of these nanomaterials with atomically thin thickness and laterally uniform dimension is essential for their promising applications in transistors, photodetectors, electroluminescent devices, catalysis, energy conversion, environment remediation, biosensing, bioimaging, and so on. Recently, the electrochemical lithium ion intercalation-based exfoliation method has emerged as a mature, efficient and promising strategy for the high-yield production of mono- or few-layer TMD nanosheets; monolayer MoS2 (yield of 92%), monolayer TaS2 (yield of 93%) and bilayer TiS2 (yield of 93%) with lateral dimensions of ~1 µm (refs. 1-3). This Protocol describes the details of experimental procedures for the high-yield synthesis of mono- or few-layer TMDs and other inorganic nanosheets such as MoS2, WS2, TiS2, TaS2, ZrS2, graphene, h-BN, NbSe2, WSe2, Sb2Se3 and Bi2Te3 by using the electrochemical lithium ion intercalation-based exfoliation method, which involves the electrochemical intercalation of lithium ions into layered inorganic crystals and a mild sonication process. The whole protocol takes 26-38 h for the successful production of ultrathin inorganic nanosheets.

Amelioration of Integrated Polyhydroxyalkanoate and Biogas Production from Waste Activated Sludge Through Mild Sonication Invoked Exopolymer Release on Thermo-Fenton Disintegration

Amelioration of Integrated Polyhydroxyalkanoate and Biogas Production from Waste Activated Sludge Through Mild Sonication Invoked Exopolymer Release on Thermo-Fenton Disintegration