Rotor-stator Mixer Research Articles

Data-driven approach for design and optimization of rotor–stator mixers for miscible fluids with different viscosities

Rotor–stator mixers (RSMs) are essential equipment used in the food, pharmaceutical, and cosmetic industries. The performance of RSMs is conventionally analyzed using three approaches based on empirical correlations and experimental and numerical analyses. This paper introduces a new approach based on a multifidelity data-driven framework for designing and optimizing RSMs that systematically combines elements of experimental and high-resolution computational fluid dynamics (CFD) models to train a machine learning model to predict RSM performance. It was subsequently coupled to an optimization solver based on a genetic algorithm. The developed framework was applied to a small-scale RSM with variable rotor blade radius, rotor speed, stator mesh width, and mass flow rate that is operated to mix two miscible fluids with different viscosities. The RSM was optimized at two regimes of low and high viscosities to achieve the best performance in terms of shaft power and mixing indices. The results demonstrate the successful application of the developed frameworks. The optimization of the mixing of high-viscosity fluids yielded a higher improvement than that for low-viscosity fluids. A decrease in shaft power of approximately 50% was obtained for the high-viscosity fluids, whereas the mixing indices increased up to 20% by the optimization of the geometrical input design parameters. The proposed framework can be advantageous for designers and operators at the industrial scale.

Numerical simulations of thixotropic semi-solid aluminium alloys in open-rotor and rotor–stator mixers

Numerical simulations of thixotropic semi-solid aluminium alloys in open-rotor and rotor–stator mixers

CFD simulation of an axial discharge rotor-stator mixer: LES versus RANS predictions

The large eddy simulation (LES) technique is used to model the turbulent flow of water in a two-stage, axial discharge, in-line rotor-stator mixer. The WALE sub-grid scale model is employed, and the resulting filtered velocity field is ensemble averaged to predict the mean velocity, turbulent kinetic energy, energy dissipation rate, and energy production rate. The results of these 3-D sliding mesh simulations are compared to analogous RANS predictions on similar meshes using the realizable k-ε turbulence model. Stator slot flow rate and rotor torque/power draw are also monitored. RANS and LES predict similar mean velocity profiles, flow rate and rotor torque. LES predicts higher turbulent kinetic energy, but lower dissipation rate compared to RANS. Results from a coarse and refined computational mesh are compared to discuss the significance of resolving smaller scales for LES. The effect of operating conditions on throughput, power draw, and other quantities of practical utility are also discussed. It was found that prediction of macroscopic quantities such as flow rate and power draw can be done efficiently using either RANS or LES on a relatively course mesh while capturing turbulence quantities requires a well refined LES simulation.

A hybrid approach based on Lagrangian particles and immersed-boundary method to characterize rotor–stator mixing systems for high viscous mixtures

In-line multi-stage rotor–stator mixing systems are the recent industrial solution for mixing highly viscous liquids in a short period of time while minimizing temperature increase throughout the mixing process. Unlike their predecessors, namely batch mixers, in-line rotor–stator mixers facilitate a continuous mode of operation. However, there is a lack of detailed insight into their flow patterns, power consumption, and mixing behavior, as these mixers, particularly the multi-stage variants, are rarely studied in the scientific community. In this work, we propose a computational framework for modeling rotor–stator mixers using Lagrangian particle tracking and the immersed-boundary method. The tracer particles present an alternative to the commonly used Eulerian approach, which is susceptible to numerical diffusion. The use of the immersed-boundary method for modeling the motion of the rotor not only significantly reduces pre-processing time but also facilitates the modeling of various rotor–stator shapes with different motion patterns, making it possible to complete the modeling in a short time. The proposed method is used to investigate an industrial in-line multi-stage rotor–stator mixer, and the accuracy of the numerical results is verified by comparing them with experimental data. The simulations unveiled that at a rotational Reynolds number of up to 4000, significant back-mixing occurs, whereas for lower Reynolds numbers, the flow maintains a smooth forward motion without any back-mixing. The study also examines the residence time of the additive in the mixer, revealing that, particularly when dealing with high-viscosity mixtures, the additive has the potential to persist in the mixer for up to 3.5 times the theoretical residence time. Additionally, the obtained results are utilized to derive empirical equations that enable predicting the mixer’s performance for different Reynolds numbers.

Triumfetta cordifolia Gum as a Promising Bio-Ingredient to Stabilize Emulsions with Potentials in Cosmetics.

The cosmetics industry is searching for efficient and sustainable substances capable of stabilizing emulsions or colloidal dispersions that are thermodynamically unstable because of their high surface energy. Therefore, surfactants are commonly used to stabilize the water/oil interface. However, the presence of a surfactant is not always sufficient to obtain stable emulsions on the one hand, and conventional surfactants are often subject to such controversies as their petroleum origin and environmental concerns on the other hand. As a consequence, among other challenges, it is obvious that research related to new-natural, biodegradable, biocompatible, available, competitive-surfactants are nowadays more intensive. This study aims to valorize a natural gum from Triumfetta cordifolia (T. cordifolia) as a sustainable emulsifier and stabilizer for oil-in-water (O/W) emulsions, and to evaluate how the nature of the fatty phase could affect this potential. To this end, O/W emulsions were prepared at room temperature using three different oils varying in composition, using a rotor-stator mixer. Resulting mixtures were characterized using optical microscopy, laser granulometry, rheology, pH and stability monitoring over time. The results demonstrated good potential for the gum as an emulsifying agent. T. cordifolia gum appears efficient even at very low concentrations (0.2% w/w) for the preparation and stabilization of the different O/W emulsions. The best results were observed for cocoglyceride oil due to its stronger effect of lowering interfacial tension (IFT) thus acting as a co-emulsifier. Therefore, overall results showed that T. cordifolia gum is undoubtedly a highly promising new bio-sourced and environmentally friendly emulsifier/stabilizer for many applications including cosmetics.

Effect of surfactants and interfacial rheology on equilibrium drop size in turbulent liquid-liquid dispersions

Surfactants are often required to stabilize liquid-liquid dispersions produced by high shear mixers. Due to the high power input, drops are deformed rapidly in the dispersion zone so the dynamic interfacial properties governed by the surfactant adsorption rate can have a significant impact on the resulting drop size. The objective of this work is to develop a fundamental link between surfactant adsorption dynamics, interfacial properties, and turbulent emulsification processes. To ensure constant bulk surfactant concentration during dispersion, equilibrium drop size for dilute dispersions produced by a batch rotor-stator mixer were studied. Silicone oils of various viscosity were dispersed in aqueous nonionic surfactant solutions. Drop size distributions (DSD) were measured via a video microscopy/automated image analysis technique. Equilibrium interfacial tension was measured via a pendant drop technique, as a function of surfactant concentration. The dynamic surface tension was similarly measured. The data were fit to the Langmuir adsorption isotherm and the long-times approximation to the Ward – Tordai equation and the adsorption parameters and surfactant diffusivities so obtained were employed, with an estimate of the drop deformation timescale, to estimate the surface dilational modulus (Esd) or Marangoni stress acting on the drop’ surface due to interfacial tension gradients. Trends observed in the measured equilibrium mean drop size and DSD are explained in terms of the interfacial and rheological properties. Below the CMC, Esd peaks and the drop size increases with bulk surfactant concentration, despite a decrease in equilibrium interfacial tension. Above the CMC, Marangoni stresses are small but the presence of the surfactant still modifies the rheology of the interface, increasing the effective viscosity of the drops. A comprehensive set of mechanistic models for drop size in turbulent flows, based on Kolmogorov-Hinze theory, was developed and modified to partially account for the effect of surfactants via an appropriately defined effective viscosity. The approach allows integration of surfactant phenomena into widely accepted correlations for drop size in surfactant free systems.

Fluid laminarization process and rheological properties of protein-stabilized high internal phase emulsions

Protein-based high internal phase emulsions (HIPEs) have gained tremendous attention in diverse fields, but their mechanism in the emulsification process remains elusive. In this article, HIPEs were stabilized directly by food-grade proteins, depending on a self-organized process featuring a fluid laminarization. We elucidated that the emulsification with the rotor-stator mixer is a typical non-equilibrium process. The crucial factor for the process is related to the irreversible energy dissipation, while the internal phase volume fraction is the threshold determining the laminarization. The feasible explanation speculated that the transition corresponds to the dissipative structure, i.e., compressive droplets, arising from the spatiotemporal self-organization, to dissipate the turbulent kinetic energy. We found a new paradigm of dissipative structure, comprehending such structure in the HIPEs emulsification process, which is expected to pave the way for its industrial-scale production with the virtue of low-cost proteins.

Influence of encapsulation variables on formation of leuprolide-loaded PLGA microspheres

Emulsion-based solvent evaporation microencapsulation methods for producing PLGA microspheres are complex often leading to empirical optimization. This study aimed to develop a more detailed understanding of the effects of process variables on the complex emulsification processes during encapsulation of leuprolide in PLGA microspheres using a high-shear rotor–stator mixer. Following extensive analysis of previously developed formulation conditions that yield microspheres of equivalent composition to the commercial 1-month Lupron Depot, multiple variables during the formation of primary and secondary emulsion were investigated with the aid of dimensional analysis, including: rotor speed (ω) and time (t), dispersed phase fraction (Φ) and continuous phase viscosity (µc). The dimensionless Sauter mean diameter (d3,2) of primary emulsion was observed to be proportional to the product of several key dimensionless groups (Φ1,We,Re,ω1t1) raised to the appropriate power indices. A new dimensionless group (Θ ) (surface energy/energy input) was used to rationalize insertion of a proportionate time dependence in the scaling of the d3,2. The dimensionless d3,2 of secondary emulsion was found proportional to the product of three dimensionless groups (Φ2,μ1′μc2,ω2t2) raised to the appropriate power indices. The increased viscosity of the primary emulsion, decreased secondary water phase volume and reduced second homogenization time each elevated encapsulation efficiency of peptide by reducing drug leakage to the outer water phase. These results could be useful for dimensional analysis and improving manufacturing of PLGA microspheres by the solvent evaporation method.

Identification and Mapping of Three Distinct Breakup Morphologies in the Turbulent Inertial Regime of Emulsification—Effect of Weber Number and Viscosity Ratio

Turbulent emulsification is an important unit operation in chemical engineering. Due to its high energy cost, there is substantial interest in increasing the fundamental understanding of drop breakup in these devices, e.g., for optimization. In this study, numerical breakup experiments are used to study turbulent fragmentation of viscous drops, under conditions similar to emulsification devices such as high-pressure homogenizers and rotor-stator mixers. The drop diameter was kept larger than the Kolmogorov length scale (i.e., turbulent inertial breakup). When varying the Weber number (We) and the disperse-to-continuous phase viscosity ratio in a range applicable to emulsification, three distinct breakup morphologies are identified: sheet breakup (large We and/or low viscosity ratio), thread breakup (intermediary We and viscosity ratio > 5), and bulb breakup (low We). The number and size of resulting fragments differ between these three morphologies. Moreover, results also confirm previous findings showing drops with different We differing in how they attenuate the surrounding turbulent flow. This can create ‘exclaves’ in the phase space, i.e., narrow We-intervals, where drops with lower We break and drops with higher We do not (due to the latter attenuating the surrounding turbulence stresses more).

Substitution of equations for evaluation of energy consumption in rotor-stator mixers

In the presented publication, an attempt to develop the theory of mixing by considering rotor-stator mixers from the standpoint of mechanical mixing devices was made.
 The results of the research on energy consumption are given in the form of analytically substituted expressions for determining power and pressure difference as well as a flow rate in a stage of rotor-stator mixer composed of a pair of the perforated rotor and stator elements with a gap between them, depending on the features of the design, dynamic characteristics of the rotor and flows. The interrelationships between power, pressure difference, and flow rate in the stages of rotor-stator mixers are established. This makes it possible to define the characteristics of mixers, carry out their calculations and reasonably accept the rational design and processing parameters. The peculiarities of the components in obtained equations are indicated. Partial cases of the equations for power consumption in stages of rotor-stator-mixers operated in pulse and impulse modes are considered. The invariant form of obtained equations would help to ease the scaling of rotor-stator mixers.

Residence time distribution and micromixing efficiency of a dynamic inline rotor–stator mixer

An industrially available dynamic inline–mixer which operates on the rotor–stator principle was investigated for aqueous solutions with a total volume flow rate of up to 40 L/h to gain valid insight into the mixing behavior. In residence time distribution (RTD) experiments, mean residence times ranging between 29 and 305 s and Bodenstein numbers ranging between 1.4 and 5.1 were measured. Micromixing efficiency was investigated with the Villermaux–Dushman reaction at varying rotational speeds, total volume flow rates and injection inlets. The results suggest that micromixing processes are especially complex in a continuous rotor–stator mixer. As expected, the injection inlet had a decisive influence on micromixing efficiency. Surprisingly, even at higher volume flow rates backmixing was identified as a factor which significantly extends the micromixing time. A new method is proposed for estimating the degree of backmixing based on micromixing experiments. Micromixing times range between 3 · 10–4 and 4 · 10–3 s depending on the operating point.

Transitioning from a lab-scale PLGA microparticle formulation to pilot-scale manufacturing.

The complexity of scale-up manufacturing of PLGA microparticles creates a significant challenge when transitioning from benchtop-scale formulation development into larger clinical scale batches. Minor changes in the initial formulation composition (e.g., PLGA molecular weight, solvent type, and drug concentration) and processing parameters (e.g., extraction kinetics and drying condition) during scale-up production can result in significantly different performance of the prepared microparticles. The objectives of the present study were to highlight the in vitro and in vivo performance of a candidate benchtop-scale batch created with a rotor-stator mixer, transitioned into an in-line manufacturing process at ~15× scale of a long-acting naltrexone formulation. Physicochemical properties (such as drug loading, residual benzyl alcohol content, and morphology) as well as the in vitro release characteristics of the prepared naltrexone microparticles between the benchtop-scale and in-line process pilot-scale were determined. The pharmacokinetics of the naltrexone microspheres were investigated using the rat model. The results demonstrate that while the morphologies of the particles were different from a visual assessment and slight differences were observed in the in vitro release profiles, the in vivo pharmacokinetics illustrate similar kinetics. Our study shows that scale-up production having the same drug release kinetics can be made by controlling the formulation and processing parameters.

A numerical study of mixing intensification for highly viscous fluids in multistage rotor–stator mixers

How to achieve uniform mixing of highly viscous fluids with low energy consumption is a major industry demand and one of the hot spots of mixing research. A typical multistage rotor–stator mixer (MRSM) equipped with a distributor was investigated to disclose the effects on the mixing performance and power consumption for highly viscous fluids via numerical simulation, considering the influence factors associated with different geometric parameters of both MRSM and the distributor. The mixing index and power consumption are used to evaluate the performance of the mixers. The dimensionless correlations for the mixing index and the power consumption are established considering the factors including the flow rate, rotor speed, the number of mixing units. Adopting the optimized mixer with the distributor (X1-T1), the mixing index increases to 0.85 (obviously higher than 0.46 for the mixer T1 without a distributor), meanwhile the corresponding power consumption is about 1/5 of that of T1 achieving the same mixing effect. It illustrates that the distributor can significantly improve the mixing of highly viscous fluids in the MRSM without the cost of large power consumption. These results would provide a guidance on the design and optimization of multistage rotor–stator mixers in industrial applications.

Preparation of Water-in-Oil Nanoemulsions Loaded with Phenolic-Rich Olive Cake Extract Using Response Surface Methodology Approach.

In this study, we aimed to prepare stable water-in-oil (W/O) nanoemulsions loaded with a phenolic-rich aqueous phase from olive cake extract by applying the response surface methodology and using two methods: rotor-stator mixing and ultrasonic homogenization. The optimal nanoemulsion formulation was 7.4% (w/w) of olive cake extract as the dispersed phase, and 11.2% (w/w) of a surfactant mixture of polyglycerol polyricinoleate (97%) and Tween 80 (3%) in Miglyol oil as the continuous phase. Optimum results were obtained by ultrasonication for 15 min at 20% amplitude, yielding W/O nanoemulsion droplets of 104.9 ± 6.7 nm in diameter and with a polydispersity index (PDI) of 0.156 ± 0.085. Furthermore, an optimal nanoemulsion with a droplet size of 105.8 ± 10.3 nm and a PDI of 0.255 ± 0.045 was prepared using a rotor-stator mixer for 10.1 min at 20,000 rpm. High levels of retention of antioxidant activity (90.2%) and phenolics (83.1–87.2%) were reached after 30 days of storage at room temperature. Both W/O nanoemulsions showed good physical stability during this storage period.

Droplet Size and Coalescence Stability of n-Hexadecane Emulsions Homogenized in Aqueous Solution of Proteins before and after High-Energy Processes

Abstract Properties of protein-based O/W emulsions are influenced by various factors including species and concentration of the protein, oil content, and employed homogenization technique, which make it difficult to establish suitable conditions to prepare stable emulsions. To address this issue, two proteins, bovine serum albumin (BSA) and ovalbumin (OVA), were used as emulsifiers in a wide concentration range to disperse n-hexadecane, and necessary conditions to prepare reasonably stable, submicron-size emulsions were explored. A two-step homogenization process, premixing with a rotor-stator mixer followed by either sonication or high-pressure homogenization, was employed, and volume-weighted average droplet diameter (d43), adsorption density of proteins (Γ), and coalescence stability of oil droplets were measured. For sonicated emulsions in the emulsifier-rich regime, d43 was ca. 1 µm for both BSA and OVA, and Γ was ca. 2–3 mg m−2 (over 15 mg m−2) for BSA (OVA). The high-pressure homogenization could reduce d43 down to 0.4 µm provided BSA (OVA) concentration was 5 g L−1 (15 g L−1) or higher. These submicron-size emulsions were stable for several days only for BSA emulsions with the concentration ≥ 15 g L−1, otherwise coalescence proceeded. These results suggested that the adsorbed OVA films are more easily broken than the BSA films.

Analysis of the Dispersion of Viscoelastic Clusters in the Industrial Rotor-Stator Equipment

Materials with complex rheology and viscoelasticity may require special equipment for processing, such as for dispergation. Rheological and mechanical data of the material can help with finding the required equipment or designing equipment. For highly viscous and complex material, a rotor-stator mixer can be a good choice for dispergation. Due to the laminar or creeping mechanism of flow inside the equipment, the dispergation mechanism is assumed to be a combination of the shear stress and slicing of the material by the rotor and stator blades. For the validation of the theory, the mechanical properties of the viscose identified in a previous work were used for comparison with the data from the CFD simulation of the rotor-stator mixer. The comparison showed that the rotor-stator device can overcome the complex shear modulus and ultimate strength of the material and homogenize the solution through a combination of the shear stress and slicing. The theory was also confirmed on the process line proposed for homogenization of the specific material. The stability of viscosity during the process of homogenization was measured and used as the main parameter for quality assessment.

The Role of Stochastic Time-Variations in Turbulent Stresses When Predicting Drop Breakup—A Review of Modelling Approaches

Many industrially relevant emulsification devices are of the high-energy type, where drop deformation and subsequent breakup, take place due to intense turbulent fluid–drop interactions. This includes high-pressure homogenizers as well as rotor-stator mixers (also known as high-shear mixers) of various designs. The stress acting on a drop in a turbulent flow field varies over time, occasionally reaching values far exceeding its time-averaged value, but only during limited stretches of time, after which it decreases down to low values again. This it is one factor separating turbulent from laminar emulsification. This contribution reviews attempts to take this intermittently time-varying stress into account in models predicting the characteristic drop diameter resulting from emulsification experiments, focusing on industrially applicable emulsification devices. Two main frameworks are discussed: the Kolmogorov–Hinze framework and the oscillatory resonance framework. Modelling suggestions are critically discussed and compared, with the intention to answer how critical it is to correctly capture this time-varying stress in emulsification modelling. The review is concluded by a list of suggestions for future investigations.

Effects of Processing Time, Mixing Speed, and Mixer on Agglomerates in Fuel Cell Cathode Inks

To prepare a catalyst ink, the large agglomerates of platinum on carbon (Pt/C) powder must be broken down into the primary aggregate particles. This physical process is necessary to form a homogenous mixture that produces uniform and defect-free coatings, as well as maximizing electrochemical performance. Large agglomerates of Pt/C catalyst can limit oxygen diffusion and reduce contact area between ionomer and active Pt area in polymer electrolyte membrane fuel cells (PEMFCs) and electrolyzer catalyst layers. Proper mixing of the catalyst ink before deposition is critical in breaking up these agglomerates, but excessive mixing wastes time and energy and, in some cases, may even damage the catalyst particles.1 There have been several studies of ultrasonication time and energy affecting cathode performance and agglomerate size.1–3 However, there has been considerably less work on mechanical mixing methods, which are more relevant for large-scale manufacturing.This work explores the impact of mixing time and speed on Pt/C agglomerate size using five different mechanical mixers including ball milling and rotor-stator mixers with distinct geometries. Optical micrograph analysis of these rod-coated catalyst layers reveals an exponential decay of particle agglomerates as a function of mixing time, eventually reaching a steady state where there is little to no change in the number of particles over 15 μm in diameter. For a given mixer geometry, mixing speed determines the lowest attainable particle size distribution with higher speeds leading to greater breakup of agglomerate particles (see Figure 1). Rheometry is utilized as a complementary technique to assess the degree of ink mixing completion. Continuous mixing renders higher ink shear viscosity values until plateauing at similar time intervals at which an unvarying particle size distribution is observed. In-situ electrochemical testing of these thin gas diffusion electrodes (GDEs) is employed to correlate the process-driven parameters that govern ink agglomerate size and rheology with fuel cell performance.This research at Oak Ridge National Laboratory, managed by UT Battelle, LLC, for the U.S. Department of Energy under contract DE- AC05-00OR22725, was sponsored by the Office of Energy Efficiency and Renewable Energy (EERE) Advanced Manufacturing Office (AMO).This work was authored in part by the National Renewable Energy Laboratory, operated by Alliance for Sustainable Energy, LLC, for the U.S. Department of Energy (DOE) under Contract No. DE-AC36-08GO28308. Funding provided by U.S. Department of Energy Office of Energy Efficiency and Renewable Energy Advanced Manufacturing Office. The views expressed in the article do not necessarily represent the views of the DOE or the U.S. Government. The U.S. Government retains and the publisher, by accepting the article for publication, acknowledges that the U.S. Government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this work, or allow others to do so, for U.S. Government purposes.(1) Wang, M.; Park, J. H.; Kabir, S.; Neyerlin, K. C.; Kariuki, N. N.; Lv, H.; Stamenkovic, V. R.; Myers, D. J.; Ulsh, M.; Mauger, S. A. Impact of Catalyst Ink Dispersing Methodology on Fuel Cell Performance Using In-Situ X-Ray Scattering. ACS Appl. Energy Mater. 2019, 2 (9), 6417–6427. https://doi.org/10.1021/acsaem.9b01037.(2) Pollet, B. G. Let’s Not Ignore the Ultrasonic Effects on the Preparation of Fuel Cell Materials. Electrocatalysis 2014, 5 (4), 330–343. https://doi.org/10.1007/s12678-014-0211-4.(3) Pollet, B. G. The Use of Ultrasound for the Fabrication of Fuel Cell Materials. Int. J. Hydrog. Energy 2010, 35 (21), 11986–12004. https://doi.org/10.1016/j.ijhydene.2010.08.021.Caption: Figure 1. Plot of number of catalyst agglomerates particles with equivalent diameter larger than 15 µm as a function of rotor-stator rotational speed and time. Figure 1

Continuous Production of Water-Based UV-Curable Polyurethane Dispersions Using Static Mixers and a Rotor-Stator Mixer.

UV-curable polyurethane dispersions (UV-PUDs) have applications in coatings for a variety of materials. Historically, the neutralization and dispersion steps of the UV-PUD production process have been performed in batch. However, continuous processing might reduce capital and operating costs, improve the dispersion characteristics, and facilitate scale-up. Static mixers and inline high-shear mixers are able to provide the necessary shear forces to obtain miniemulsions. The production of a UV-PUD is therefore studied in a continuous setup, whereby the neutralization step is performed in static mixers and the dispersion step is performed either in static mixers or in a high-shear mixer. The influence of the prepolymer temperature, mixing energy, and feed flow rate on the particle size and stability of the UV-PUD particles in water is explored. The results show that the neutralization step is mixing-sensitive, and the temperature of the neutralized prepolymer influences the particle size in the dispersion process. The amount of shear force applied during the dispersion step has a limited effect on the particle size. UV-PU dispersions with an average particle size below 80 nm and PDI below 0.1 are obtained with static mixers or in an inline rotor-stator mixer, at flow rates of 5.2 and 7.2 L/h, respectively. This research demonstrates that continuous processing using static mixers and high-shear mixing is a viable option for the neutralization and dispersion of UV-PUDs.

Very-few-layer graphene obtained from facile two-step shear exfoliation in aqueous solution

A defect-free graphene with 1–3 layers (very-few-layer graphene, VFLG) has been successfully produced using a facile and environmentally friendly two-step shear exfoliation method in rotating-blade mixer (kitchen blender) and in high shear rotor–stator mixer. An aqueous solution containing an inexpensive and safe anionic surfactant of sodium lauryl sulphate (SLS) was deployed as the working fluid. Raman spectroscopy (RS) and Raman imaging (RI), density functional theory (DFT) simulation, transmission electron microscopy and high-resolution transmission electron microscopy (TEM-HRTEM), as well as Fourier-transform infrared spectroscopy (FTIR) analyses were used to characterize the samples. Some configurations of mixer setting were applied, and the exfoliation mechanisms were discussed. RS analysis revealed that the exfoliation process in rotating-blade mixer continued by high shear in rotor–stator mixer for 3 h had produced VFLG dominated by a single layer of graphene. The Lorentzian peak fitting of 2D band was well-fitted by a single Lorentzian component at Raman shift of 2651.317 cm−1. The produced VFLG endured the lowest peak intensity ratio of D and G bands (ID/IG) of 0.146 which corresponded with the highest lateral size. RI analysis showed that produced VFLG had edge chirality of armchairs and zigzag terminations. TEM-HRTEM confirmed the presence of VFLG with the highest mean lateral size of ~375.4 nm. DFT calculations provided pertinent optical/electronic properties of graphene in terms of Raman Spectra, density of states (DOS) curve and nuclear magnetic resonance (NMR) shielding tensor. FTIR analysis showed that the exfoliation process did not cause any oxidation, sulphonation, or functional defects on the VFLG. The turbulence and hydrodynamic force in liquid were the critical factors in the exfoliation processes. High-quality VFLG, with a facile, inexpensive, and environmentally friendly synthesis process, rendered this process to be a promising route for large-scale high-quality graphene production.