Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten  Disulfide Nanotubes

Raichman, Daniel; Strawser, David; Lellouche, Jean‐Paul

doi:10.3390/inorganics2030455

Cited by 5 publications

(5 citation statements)

References 16 publications

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“…Realizing the important ramifications of this new derivatization method, we undertook in parallel with the present study an optimization study [50], via design of experiments (DoE) methodology of several reaction parameters to maximize the yield of polyCOOH f-INT-WS 2 . In addition to finding optimum values of reaction factors, an interaction analysis indicated that reaction parameters might be adjusted to tune the level of poly-carboxylation obtained.…”

Section: Introductionmentioning

confidence: 99%

Covalent functionalization/polycarboxylation of tungsten disulfide inorganic nanotubes (INTs-WS2)

2014

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KEYWORDStungsten disulfide nanotubes, inorganic nanotube of tungsten disulfide (INT-WS 2 ), Vilsmeier-Haack reagents, polycarboxylation, inorganic nanotube functionalization ABSTRACT Inorganic nanotubes of tungsten disulfide (INTs-WS 2 ) are insoluble in common solvents and practically inert, hindering their usefulness in both research and commercial applications. The covalent attachment of functional species onto the surface of INT-WS 2 is a critical first step in realizing the potential that INT-WS 2 offer for high-performance materials and products. Although a few attempts have been reported regarding preparing modified nanotubes, only a limited range of surface functionalities is possible with these methods. We have developed a versatile method, based on a modified, highly electrophilic acidic VilsmeierHaack reagent, to produce covalently bonded, polycarboxylated functional WS 2 nanotubes that are dispersible in polar liquids, including water. The surface polycarboxylated shell provides a means for additional derivatization, enabling matching compatibility of derivatized nanotubes to both hydrophobic and hydrophilic materials. Nanocomposites incorporating derivatized INT-WS 2 are expected to show improved properties as a result of enhanced interfacial compatibility, made possible by the large number of classes of functionalization available through the initial polycarboxylation step.

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Section: Introductionmentioning

confidence: 99%

Covalent functionalization/polycarboxylation of tungsten disulfide inorganic nanotubes (INTs-WS2)

2014

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“…This functionalization method was optimized by the design-of-experiment (DoE) methodology. [ 26 ] This method is included, along with the method described in this paper and with other functionalization methods developed in our group, in a U.S. provisional patent application. [ 27 ] In this paper, we present a new method for the functionalization of WS 2 INTs with conformal, humin-like coatings of different thicknesses.…”

Section: Introductionmentioning

confidence: 99%

“…These iminium salts are electrophilic species that can be attacked by the surface sulfur atoms of the WS 2 INTs. This functionalization method was optimized by the design‐of‐experiment (DoE) methodology . This method is included, along with the method described in this paper and with other functionalization methods developed in our group, in a U.S. provisional patent application…”

Section: Introductionmentioning

confidence: 99%

Functionalization of Tungsten Disulfide Nanotubes with a Conformal Humin‐Like Shell

Sade

Lellouche

2016

Adv Materials Inter

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Nanostructures of transition metal dichalcogenides (TMDs) exhibit excellent tribological and mechanical properties. These properties account for the intensive study of their use as additives to polymeric matrices. Functionalization of TMD nanostructures with organic chemical moieties has not yet been widely researched. Functionalization of this nature improves the ability to integrate TMD nanostructures in such matrices. In this paper, a new method for the functionalization of WS 2 inorganic nanotubes (INTs) with a conformal humin-like shell in different thicknesses is presented. The method is based on Lewis acid-activated thioglycosylation chemistry between the nanotube surface and the carbohydrate unit. It is shown that shell thickness can be controlled by adjusting the sugar concentration. A reaction between the functionalized nanotubes and 3-aminopropyl-triethoxysilane (APTES), an amineterminated silicate, for the addition of different surface functionalities is proposed. This pathway should help improve and expand the range of TMD nanostructure applications.

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“…However, in many cases, the adhesion between a nanoparticle and the polymer matrix is limited to the weak van der Waals interaction and could be enhanced by means of covalent bonding at the nanoparticle-polymer interface. Surface functionalization of IFs or INTs, as reported by Raichmann et al [10], could provide stronger adhesion of nanoparticles with the polymer matrix. The emphasis in this direction was given to the non-trivial functionalization of the hydrophobic WS2 nanotubes by hydrophilic carboxyl groups, which could further stimulate the fabrication of hydrophilic polymer composites or ceramics.…”

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confidence: 87%

Inorganic Fullerene-Like Nanoparticles and Inorganic Nanotubes

Tenne

Enyashin

2014

Inorganics

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Fullerene-like nanoparticles (inorganic fullerenes; IF) and nanotubes of inorganic layered compounds (inorganic nanotubes; INT) combine low dimensionality and nanosize, enhancing the performance of corresponding bulk counterparts in their already known applications, as well as opening new fields of their own [1]. This issue gathers articles from the diverse area of materials science and is devoted to fullerene-like nanoparticles and nanotubes of layered sulfides and boron nitride and collects the most current results obtained at the interface between fundamental research and engineering. Arising from fortuitous lab discovery, the commercial production of inorganic hollow nanoparticles was focused on molybdenum and tungsten disulfides. Their superior solid lubrication effects have engendered intense industrial scale-up and commercialization, with sales of thousands of tons of formulated lubricants per year [2]. One of the papers of this issue describes an attempt for further rationalization and scale-up of the manufacturing of WS2 nanoparticles after gas-solid reductive sulfurization of WO3 nanoparticles in a rotary furnace [3]. This systematic study included the investigation of many reaction parameters such as precursor type, reaction temperature and time, and the reducing atmosphere. This new technique could, in the future, become a successful alternative for increasing the yield of IF production compared to the current fluidized-bed reactor. The fullerene-like morphology of MoS2 and WS2 considerably improves the tribological properties of these compounds, pushing ahead the large-scale use of layered sulfides in machinery, aerospace and in the future also in medical industries as dry and oil-based lubricants as well as wear-resistant surface

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Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes

Cited by 5 publications

References 16 publications

Covalent functionalization/polycarboxylation of tungsten disulfide inorganic nanotubes (INTs-WS2)

Covalent functionalization/polycarboxylation of tungsten disulfide inorganic nanotubes (INTs-WS2)

Functionalization of Tungsten Disulfide Nanotubes with a Conformal Humin‐Like Shell

Inorganic Fullerene-Like Nanoparticles and Inorganic Nanotubes

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