The sequential continuous-flow hydrothermal synthesis of molybdenum disulphide

Dunne, Peter W.; Munn, Alexis S.; Starkey, Chris L.; Lester, Edward

doi:10.1039/c4cc10158h

Cited by 34 publications

(28 citation statements)

References 20 publications

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“…Microwave hydrothermal and solvothermal synthesis count as ones of the most popular methods of obtaining nanomaterials [56,57]. They are systematically developed by constructing new types of reactors, for example, stop-flow and continuous-flow ones [58][59][60][61][62][63].…”

Section: Introductionmentioning

confidence: 99%

Effect of Water Content in Ethylene Glycol Solvent on the Size of ZnO Nanoparticles Prepared Using Microwave Solvothermal Synthesis

Wojnarowicz

Opalińska

Chudoba

et al. 2016

Journal of Nanomaterials

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Zinc oxide nanoparticles (ZnO NPs) were obtained by the microwave solvothermal synthesis (MSS) method. The precursor of the MSS reaction was a solution of hydrated zinc acetate in ethylene glycol with water addition. It was proved that by controlling the water concentration in the precursor it was possible to control the size of ZnO NPs in a programmed manner. The less the water content in the precursor, the smaller the size of ZnO NPs obtained. The obtained NPs with the average particle size ranging from 25 nm to 50 nm were characterised by homogeneous morphology and a narrow distribution of particle sizes. The following parameters of the obtained ZnO NPs were determined: pycnometric density, specific surface area, phase purity, chemical composition, lattice parameters, average particle size, and particle size distribution. The average size of ZnO NPs was determined using Scherrer’s formula, Nanopowder XRD Processor Demo web application, by converting the results of the specific surface area, and TEM tests using the dark field technique. ZnO morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The test performed by the X-ray powder diffraction (XRD) confirmed that crystalline ZnO, pure in terms of phase, had been obtained.

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Section: Introductionmentioning

confidence: 99%

Effect of Water Content in Ethylene Glycol Solvent on the Size of ZnO Nanoparticles Prepared Using Microwave Solvothermal Synthesis

Wojnarowicz

Opalińska

Chudoba

et al. 2016

Journal of Nanomaterials

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“…However, over the last 10 years, researchers have had considerable success synthesizing a wider range of materials, including metals [14], spinel materials [15], sulfides [16,17], hydroxides [18,19], phosphates [20], nitrides [21], and more complex materials such as metal organic frameworks [22]. Figure 1 shows a range of particles from metals to oxides to sulfides that were synthesized during the SHYMAN project, which funded this research work.…”

Section: Introductionmentioning

confidence: 99%

Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation

et al. 2016

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(2016) Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation. Nano Research, 9 (11). pp. 3377-3387. ISSN 1998-0000 Access from the University of Nottingham repository: http://eprints.nottingham.ac.uk/41016/1/1215_proof.pdf Copyright and reuse:The Nottingham ePrints service makes this work by researchers of the University of Nottingham available open access under the following conditions. This article is made available under the University of Nottingham End User licence and may be reused according to the conditions of the licence. For more details see: http://eprints.nottingham.ac.uk/end_user_agreement.pdf A note on versions:The version presented here may differ from the published version or from the version of record. If you wish to cite this item you are advised to consult the publisher's version. Please see the repository url above for details on accessing the published version and note that access may require a subscription. ABSTRACTContinuous hydrothermal synthesis was highlighted in a recent review as an enabling technology for the production of nanoparticles. In recent years, it has been shown to be a suitable reaction medium for the synthesis of a wide range of nanomaterials. Many single and complex nanomaterials such as metals, metal oxides, doped oxides, carbonates, sulfides, hydroxides, phosphates, and metal organic frameworks can be formed using continuous hydrothermal synthesis techniques. This work presents a methodology to characterize continuous hydrothermal flow systems both experimentally and numerically, and to determine the scalability of a counter current supercritical water reactor for the large scale production (>1,000 T•year -1 ) of nanomaterials. Experiments were performed using a purpose-built continuous flow rig, featuring an injection loop on a metal salt feed line, which allowed the injection of a chromophoric tracer. At the system outlet, the tracer was detected using UV/Vis absorption, which could be used to measure the residence time distribution within the reactor volume. Computational fluid dynamics (CFD) calculations were also conducted using a modeled geometry to represent the experimental apparatus. The performance of the CFD model was tested against experimental data, verifying that the CFD model accurately predicted the nucleation and growth of the nanomaterials inside the reactor.

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“…CVD offers high quality MoS 2 nanosheets, but the methodology is quite expensive and offers low productivity. The first continuous hydrothermal flow synthesis of MoS 2 was reported by Dunne and co‐workers in 2015 where MoS 2 nanosheets were produced by sulfidation of molybdate anions and in flow acidification to amorphous MoS 3 which transformed into MoS 2 nanosheets on further hydrothermal treatment …”

Section: Two‐dimensional (2d) Materials and Propertiesmentioning

confidence: 99%

Chemical Functionalisation of 2D Materials by Batch and Continuous Hydrothermal Flow Synthesis

Alli

Hettiarachchi

Kellici

2020

Chemistry A European J

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2D materials are single or few layered materials consisting of one or several elements with a thickness of a few nanometres. Their unique, tuneable physical and chemical properties including ease of chemical functionalisation makes this class of materials useful in a variety of technological applications. The feasibility of 2D materials strongly depends on better synthetic approaches to improve properties, increase performance, durability and reduce costs. As such, in the synthesis of nanomaterials, hydrothermal processes are widely adopted through a precursor–product synthesis route. This method includes batch or continuous flow systems, both employing water at elevated temperatures (above boiling point) and pressures to fine‐tune the physical, chemical, optical and electronic properties of the nanomaterial. Both techniques yield particles with different morphology, size and surface area due to different mechanisms of particle formation. In this Minireview, we present batch and continuous hydrothermal flow synthesis of a selection of 2D derivatives (graphene, MXene and molybdenum disulfide), their chemical functionalisation as an advantageous approach in exploring properties of these materials as well as the benefits and challenges of employing these processes, and an outlook for further research.

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The sequential continuous-flow hydrothermal synthesis of molybdenum disulphide

Cited by 34 publications

References 20 publications

Effect of Water Content in Ethylene Glycol Solvent on the Size of ZnO Nanoparticles Prepared Using Microwave Solvothermal Synthesis

Effect of Water Content in Ethylene Glycol Solvent on the Size of ZnO Nanoparticles Prepared Using Microwave Solvothermal Synthesis

Understanding bottom-up continuous hydrothermal synthesis of nanoparticles using empirical measurement and computational simulation

Chemical Functionalisation of 2D Materials by Batch and Continuous Hydrothermal Flow Synthesis

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