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Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes

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A special issue of Inorganics (ISSN 2304-6740). This special issue belongs to the section "Inorganic Solid-State Chemistry".

Deadline for manuscript submissions: closed (15 March 2014) | Viewed by 86702

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Prof. Dr. Reshef Tenne

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Department of Materials and Interfaces, Weizmann Institute, Rehovot 76100, Israel
Interests: nanoparticles synthesis; solid state chemistry; characterization of nanoparticles
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Dr. Andrey N. Enyashin

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Institute of Solid State Chemistry UB RAS, Pervomayskaya Str. 91, 620990 Ekaterinburg, Russia
Interests: computational materials science; inorganic fullerenes and nanotubes; carbon nanostructures

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Dear Colleagues,

Inorganic fullerene-like nanoparticles and inorganic nanotubes represent a relatively new type of condensed matter. They are constructed from non-carbon layers that are folded into tubular, polyhedral or quasi-spherical shells. This combination of low dimensionality and nano-size can enhance the layered compounds’ performance in their already known applications, as well as in new fields of use. The production of inorganic hollow nanoparticles initially arose in the 1990’s from a fortuitous lab discovery of a great number of fullerenic and nanotubular chalco- and halogenides. Commercial production of said particles now focuses on molybdenum and tungsten disulfides; tons per year are currently synthesized. MoS₂ and WS₂ are well established dry lubricants. The tribological characteristics and stability of these lubricants can be considerably enhanced by taking advantage of fullerene-like morphologies. Moreover, nanotubes and fullerene-like MoS₂ and WS₂ can be functionalized so as to transfer their excellent properties to oil-based lubricants and wear-resistant surface coatings, thus pushing ahead the large-scale use of layered sulfides in the machinery, aerospace, and medical industries. Apart from tribological qualities, the significant stability of sulfide fullerene-like nanoparticles and nanotubes under shock-wave propagation suggests their potential as fillers for impact resilient polymer or ceramic composites.

Substantial progress in the warrantable production and pioneering use of this kind of inorganic nanomaterials was possible due to comprehensive basic research on their formation mechanism, chemical reactivities, and mechanical and electronic characteristics. However, current experimental work has rapidly advanced in the direction of targeted functionalization of the nanoparticles using doping, intercalation, surface modification by molecules, endohedral sealing. Furthermore, various polymer nanocomposites containing minute amounts of these nanoparticles were shown to exhibit enhanced mechanical properties (reinforcement).The optical and electronic transport properties have been recently studied in some cases. Although the primary emphasis has been placed on molybdenum and tungsten disulfide species, the mass fabrication of BN nanotubes and the potential strategies for extended production of various other fullerene-like nanoparticles (BN, ReS₂, LnF₃ etc.) has also been demonstrated. Novel and modified nanoparticles can provide for a much larger diversity of new nanomaterials in catalysis, electronics and electrochemistry; however, the detailed characterization of such particles is required. Despite some success in the description of polyhedral fullerenes’ construction principles, understanding the morphology of fullerene-like nanoparticles at the atomistic level is still a challenge from both theoretical and experimental perspectives. The exact formation mechanisms, the interface phenomena, along with the details of mechanical destruction of the inorganic hollow nanoparticles under load, are still poorly described or remain unknown in most of the cases.

Therefore, this special issue welcomes comprehensive reviews and research articles to collect the widest information available to date in the field of inorganic fullerene-like nanoparticles and nanotubes.

Prof. Dr. Reshef Tenne
Dr. Andrey N. Enyashin
Guest Editors

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Editorial

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174 KiB

Open AccessEditorial

Inorganic Fullerene-Like Nanoparticles and Inorganic Nanotubes

by Reshef Tenne and Andrey N. Enyashin

Inorganics 2014, 2(4), 649-651; https://doi.org/10.3390/inorganics2040649 - 28 Nov 2014

Cited by 6 | Viewed by 4774

Abstract

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.[...] Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

Research

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554 KiB

Open AccessArticle

Noble-Metal Chalcogenide Nanotubes

by Nourdine Zibouche, Agnieszka Kuc, Pere Miró and Thomas Heine

Inorganics 2014, 2(4), 556-564; https://doi.org/10.3390/inorganics2040556 - 24 Oct 2014

Cited by 6 | Viewed by 5880

Abstract

We explore the stability and the electronic properties of hypothetical noble-metal chalcogenide nanotubes PtS₂, PtSe₂, PdS₂ and PdSe₂ by means of density functional theory calculations. Our findings show that the strain energy decreases inverse quadratically with the tube diameter, as is typical for other nanotubes. Moreover, the strain energy is independent of the tube chirality and converges towards the same value for large diameters. The band-structure calculations show that all noble-metal chalcogenide nanotubes are indirect band gap semiconductors. The corresponding band gaps increase with the nanotube diameter rapidly approaching the respective pristine 2D monolayer limit. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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5406 KiB

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

by Daniel Raichman, David Strawser and Jean-Paul Lellouche

Inorganics 2014, 2(3), 455-467; https://doi.org/10.3390/inorganics2030455 - 11 Aug 2014

Cited by 5 | Viewed by 5351

Abstract

Design of experiments (DOE) methodology was used to identify and optimize factors that influence the degree of functionalization (polycarboxylation) of WS₂ INTs via a modified acidic Vilsmeier–Haack reagent. The six factors investigated were reaction time, temperature and the concentrations of 2-bromoacetic acid, WS₂ INTs, silver acetate and DMF. The significance of each factor and the associated interactive effects were evaluated using a two-level factorial statistical design in conjunction with statistical software (MiniTab^® 16) based on quadratic programming. Although statistical analysis indicated that no factors were statistically significant, time, temperature and concentration of silver acetate were found to be the most important contributors to obtaining maximum functionalization/carboxylation. By examining contour plots and interaction plots, it was determined that optimal functionalization is obtained in a temperature range of 115–120 °C with a reaction time of 54 h using a mixture of 6 mL DMF, 200 mg INTs, 800 mg 2-bromoacetic acid and 60 mg silver acetate. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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6301 KiB

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Microstructural Study of IF-WS₂ Failure Modes

by Jamie Cook, Steven Rhyans, Lou Roncase, Garth Hobson and Claudia C. Luhrs

Inorganics 2014, 2(3), 377-395; https://doi.org/10.3390/inorganics2030377 - 04 Jul 2014

Cited by 8 | Viewed by 6295

Abstract

This manuscript summarizes the failure mechanisms found in inorganic fullerene-type tungsten disulfide (IF-WS₂) nanoparticles treated with diverse pressure loading methods. The approaches utilized to induce failure included: the use of an ultrasonic horn, the buildup of high pressures inside a shock tube which created a shock wave that propagated and impinged in the sample, and impact with military rounds. After treatment, samples were characterized using electron microscopy, powder X-ray diffraction, energy dispersive X-ray spectroscopy, and surface area analysis. The microstructural changes observed in the IF-WS₂ particulates as a consequence of the treatments could be categorized in two distinct fracture modes. The most commonly observed was the formation of a crack at the particles surface followed by a phase transformation from the 3D cage-like structures into the 2D layered polymorphs, with subsequent agglomeration of the plate-like sheets to produce larger particle sizes. The secondary mechanism identified was the incipient delamination of IF-WS₂. We encountered evidence that the IF-WS₂ structure collapse initiated in all cases at the edges and vertices of the polyhedral particles, which acted as stress concentrators, independent of the load application mode or its duration. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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1516 KiB

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The Role of Lead (Pb) in the High Temperature Formation of MoS₂ Nanotubes

by Olga Brontvein, Reshef Tenne and Andrey Enyashin

Inorganics 2014, 2(2), 363-376; https://doi.org/10.3390/inorganics2020363 - 23 Jun 2014

Cited by 8 | Viewed by 4508

Abstract

Recent studies have clearly indicated the favorable effect of lead as a growth promoter for MX₂ (M = Mo, W; X = S, Se) nanotubes using MX₂ powder as a precursor material. The experimental work indicated that the lead atoms are not stable in the molybdenum oxide lattice ion high concentration. The initial lead concentration in the oxide nanowhiskers (Pb:Mo ratio = 0.28) is reduced by one order of magnitude after one year in the drawer. The initial Pb concentration in the MoS₂ nanotubes lattice (produced by solar ablation) is appreciably smaller (Pb:Mo ratio for the primary samples is 0.12) and is further reduced with time and annealing at 810 °C, without consuming the nanotubes. In order to elucidate the composition of these nanotubes in greater detail; the Pb-“modified” MX₂ compounds were studied by means of DFT calculations and additional experimental work. The calculations indicate that Pb doping as well as Pb intercalation of MoS₂ lead to the destabilization of the system; and therefore a high Pb content within the MoS₂ lattice cannot be expected in the final products. Furthermore; substitutional doping (Pb_Mo) leads to p-type semiconducting character; while intercalation of MoS₂ by Pb atoms (Pb_y/MoS₂) should cause n-type semiconducting behavior. This study not only sheds light on the role of added lead to the growth of the nanotubes and their role as electron donors; but furthermore could pave the way to a large scale synthesis of the MoS₂ nanotubes. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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4143 KiB

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Gas-Phase and Microsolvated Glycine Interacting with Boron Nitride Nanotubes. A B3LYP-D2* Periodic Study

by Albert Rimola and Mariona Sodupe

Inorganics 2014, 2(2), 334-350; https://doi.org/10.3390/inorganics2020334 - 18 Jun 2014

Cited by 15 | Viewed by 5950

Abstract

The adsorption of glycine (Gly) both in gas-phase conditions and in a microsolvated state on a series of zig-zag (n,0) single-walled boron nitride nanotubes (BNNTs, n = 4, 6, 9 and 15) has been studied by means of B3LYP-D2* periodic calculations. Gas-phase Gly is found to be chemisorbed on the (4,0), (6,0) and (9,0) BNNTs by means of a dative interaction between the NH₂ group of Gly and a B atom of the BNNTs, whose computed adsorption energies are gradually decreased by increasing the tube radius. On the (15,0) BNNT, Gly is found to be physisorbed with an adsorption driving force mainly dictated by p-stacking dispersion interactions. Gly adsorption in a microsolvated environment has been studied in the presence of seven water molecules by progressively microsolvating the dry Gly/BNNT interface. The most stable structures on the (6,0), (9,0) and (15,0) BNNTs present the Gly/BNNT interface fully bridged by the water solvent molecules; i.e., no direct contact between Gly and the BNNTs takes place, whereas on the (4,0) BNNT the most stable structure presents a unique direct interaction between the COO⁻ Gly group and a B atom of the nanotube. Further energetic analyses indicate that the (6,0), (9,0) and (15,0) BNNTs exhibit a low water affinity, which favors the Gly/water interactions upon BNNT coadsorption. In contrast, the (4,0) BNNT has been found to show a large water affinity, bringing the replacement of adsorbed water by a microsolvated glycine molecule as an unfavorable process. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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6070 KiB

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Continuous Production of IF-WS₂ Nanoparticles by a Rotary Process

by Fang Xu, Nannan Wang, Hong Chang, Yongde Xia and Yanqiu Zhu

Inorganics 2014, 2(2), 313-333; https://doi.org/10.3390/inorganics2020313 - 13 Jun 2014

Cited by 17 | Viewed by 8899

Abstract

This manuscript demonstrates the design, modification and initial investigation of a rotary furnace for the manufacturing of inorganic fullerene WS₂ nanoparticles. Different preparation methods starting with various precursors have been investigated, of which the gas-solid reaction starting with WO₃ nanoparticles was the most efficient technique. Furthermore, the influence of temperature, reaction time, and reaction gases etc. on the synthesis of inorganic fullerene WS₂ nanomaterials was investigated, and these parameters were optimised based on combined characterisations using XRD, SEM and TEM. In addition, the furnace was further modified to include a baffled tube, a continuous gas-blow feeding system, and a collection system, in order to improve the batch yield and realise continuous production. This technique has improved the production from less than 1 g/batch in a traditional tube furnace to a few tens of g/batch, and could be easily scaled up to industry level production. Full article

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1843 KiB

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Thermoplastic Polymer Nanocomposites Based on Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes

by Mohammed Naffakh and Ana M. Díez-Pascual

Inorganics 2014, 2(2), 291-312; https://doi.org/10.3390/inorganics2020291 - 12 Jun 2014

Cited by 52 | Viewed by 8406

Abstract

Using inorganic fullerene-like (IF) nanoparticles and inorganic nanotubes (INT) in organic-inorganic hybrid composite, materials provide the potential for improving thermal, mechanical, and tribological properties of conventional composites. The processing of such high-performance hybrid thermoplastic polymer nanocomposites is achieved via melt-blending without the aid of any modifier or compatibilizing agent. The incorporation of small quantities (0.1–4 wt.%) of IF/INTs (tungsten disulfide, IF-WS₂ or molybdenum disulfide, MoS₂) generates notable performance enhancements through reinforcement effects and excellent lubricating ability in comparison with promising carbon nanotubes or other inorganic nanoscale fillers. It was shown that these IF/INT nanocomposites can provide an effective balance between performance, cost effectiveness, and processability, which is of significant importance for extending the practical applications of diverse hierarchical thermoplastic-based composites. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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1220 KiB

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From Stable ZnO and GaN Clusters to Novel Double Bubbles and Frameworks

by Matthew R. Farrow, John Buckeridge, C. Richard A. Catlow, Andrew J. Logsdail, David O. Scanlon, Alexey A. Sokol and Scott M. Woodley

Inorganics 2014, 2(2), 248-263; https://doi.org/10.3390/inorganics2020248 - 28 May 2014

Cited by 10 | Viewed by 5237

Abstract

A bottom up approach is employed in the design of novel materials: first, gas-phase “double bubble” clusters are constructed from high symmetry, T_h, 24 and 96 atom, single bubbles of ZnO and GaN. These are used to construct bulk frameworks. Upon geometry optimization—minimisation of energies and forces computed using density functional theory—the symmetry of the double bubble clusters is reduced to either C₁ or C₂, and the average bond lengths for the outer bubbles are 1.9 Å, whereas the average bonds for the inner bubble are larger for ZnO than for GaN; 2.0 Å and 1.9 Å, respectively. A careful analysis of the bond distributions reveals that the inter-bubble bonds are bi-modal, and that there is a greater distortion for ZnO. Similar bond distributions are found for the corresponding frameworks. The distortion of the ZnO double bubble is found to be related to the increased flexibility of the outer bubble when composed of ZnO rather than GaN, which is reflected in their bulk moduli. The energetics suggest that (ZnO)₁₂@(GaN)₄₈ is more stable both in gas phase and bulk frameworks than (ZnO)₁₂@(ZnO)₄₈ and (GaN)₁₂@(GaN)₄₈. Formation enthalpies are similar to those found for carbon fullerenes. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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7686 KiB

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IF-WS₂/Nanostructured Carbon Hybrids Generation and Their Characterization

by Claudia C. Luhrs, Michael Moberg, Ashley Maxson, Luke Brewer and Sarath Menon

Inorganics 2014, 2(2), 211-232; https://doi.org/10.3390/inorganics2020211 - 09 May 2014

Cited by 29 | Viewed by 9278

Abstract

With the aim to develop a new generation of materials that combine either the known energy absorbing properties of carbon nanofibers (CNF), or the carbon-carbon bond strength of graphene sheets (G), with the shock resistance properties reported for Inorganic Fullerene type WS₂ structures (IF-WS₂), hybrid CNF/IF-WS₂and G/IF-WS₂were generated, characterized and tested. Experimentation revealed that in situ growth of carbon nanostructures with inorganic fullerene tungsten disulfide particulates had to be performed from particular precursors and fabrication conditions to avoid undesirable byproducts that hinder fiber growth or deter graphene generation. The novel protocols that allowed us to integrate the IF-WS₂ with the carbon nanostructures, producing dispersions at the nanoscale, are reported. Resulting hybrid CNF/IF-WS₂and G/IF-WS₂products were analyzed by X-ray Diffraction (XRD), Scanning Electron Microscope (SEM) and TEM (Transmission Electron Microscopy). The thermal stability of samples in air was evaluated by Thermogravimetric Analysis (TGA). CNF/IF-WS₂and G/IF-WS₂hybrids were introduced into epoxy matrices, and the mechanical properties of the resulting composites were analyzed using nanoindentation. Epoxy composite samples showed drastic improvements in the Young’s modulus and hardness values by the use of only 1% hybrid weight loadings. The carbon nanofiber inclusions seem to have a much greater impact on the mechanical properties of the composite than the graphene based counterparts. Full article

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9363 KiB

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Single- to Triple-Wall WS₂ Nanotubes Obtained by High-Power Plasma Ablation of WS₂ Multiwall Nanotubes

by Volker Brüser, Ronit Popovitz-Biro, Ana Albu-Yaron, Tommy Lorenz, Gotthard Seifert, Reshef Tenne and Alla Zak

Inorganics 2014, 2(2), 177-190; https://doi.org/10.3390/inorganics2020177 - 29 Apr 2014

Cited by 26 | Viewed by 7345

Abstract

The synthesis of inorganic nanotubes (INT) from layered compounds of a small size (<10 nm in diameter) and number of layers (<4) is not a trivial task. Calculations based on density functional tight-binding theory (DFTB) predict that under highly exergonic conditions, the reaction could be driven into a “window” of (meta-) stability, where 1–3-layer nanotubes will be formed. Indeed, in this study, single- to triple-wall WS₂ nanotubes with a diameter of 3–7 nm and a length of 20–100 nm were produced by high-power plasma irradiation of multiwall WS₂ nanotubes. As target materials, plane crystals (2H), quasi spherical nanoparticles (IF) and multiwall, 20–30 layers, WS₂nanotubes were assessed. Surprisingly, only INT-WS₂ treated by plasma resulted in very small, and of a few layers, “daughter” nanotubules. The daughter nanotubes occur mostly attached to the outer surface of the predecessor, i.e., the multiwall “mother” nanotubes. They appear having either a common growth axis with the multiwall nanotube or tilted by approximately 30° or 60° with respect to its axis. This suggests that the daughter nanotubes are generated by exfoliation along specific crystallographic directions. A growth mechanism for the daughter nanotubes is proposed. High resolution transmission and scanning electron microscopy (HRTEM/HRSEM) analyses revealed the distinctive nanoscale structures and helped elucidating their growth mechanism. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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814 KiB

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Electromechanical Properties of Small Transition-Metal Dichalcogenide Nanotubes

by Nourdine Zibouche, Mahdi Ghorbani-Asl, Thomas Heine and Agnieszka Kuc

Inorganics 2014, 2(2), 155-167; https://doi.org/10.3390/inorganics2020155 - 23 Apr 2014

Cited by 19 | Viewed by 5852

Abstract

Transition-metal dichalcogenide nanotubes (TMC-NTs) are investigated for their electromechanical properties under applied tensile strain using density functional-based methods. For small elongations, linear strain-stress relations according to Hooke’s law have been obtained, while for larger strains, plastic behavior is observed. Similar to their 2D counterparts, TMC-NTs show nearly a linear change of band gaps with applied strain. This change is, however, nearly diameter-independent in case of armchair forms. The semiconductor-metal transition occurs for much larger deformations compared to the layered tube equivalents. This transition is faster for heavier chalcogen elements, due to their smaller intrinsic band gaps. Unlike in the 2D forms, the top of valence and the bottom of conduction bands stay unchanged with strain, and the zigzag NTs are direct band gap materials until the semiconductor-metal transition. Meanwhile, the applied strain causes modification in band curvature, affecting the effective masses of electrons and holes. The quantum conductance of TMC-NTs starts to occur close to the Fermi level when tensile strain is applied. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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Review

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Nanostructured Boron Nitride: From Molecular Design to Hydrogen Storage Application

by Georges Moussa, Chrystelle Salameh, Alina Bruma, Sylvie Malo, Umit B. Demirci, Samuel Bernard and Philippe Miele

Inorganics 2014, 2(3), 396-409; https://doi.org/10.3390/inorganics2030396 - 31 Jul 2014

Cited by 21 | Viewed by 7750

Abstract

The spray-pyrolysis of borazine at 1400 °C under nitrogen generates boron nitride (BN) nanoparticles (NPs). The as-prepared samples form elementary blocks containing slightly agglomerated NPs with sizes ranging from 55 to 120 nm, a Brunauer-Emmett-Teller (BET)-specific surface area of 34.6 m² g⁻¹ and a helium density of 1.95 g cm⁻³. They are relatively stable in air below 850 °C in which only oxidation of the NP surface proceeds, whereas under nitrogen, their lower size affects their high temperature thermal behavior in the temperature range of 1450–2000 °C. Nitrogen heat-treated nanostructures have been carefully analyzed using X-ray diffraction, electron microscopy and energy-dispersive X-ray spectroscopy. The high temperature treatment (2000 °C) gives hollow-cored BN-NPs that are strongly facetted, and after ball-milling, hollow core-mesoporous shell NPs displaying a BET-specific surface area of 200.5 m²·g⁻¹ and a total pore volume of 0.287 cm³·g⁻¹ were produced. They have been used as host material to confine, then destabilize ammonia borane (AB), thus improving its dehydrogenation properties. The as-formed AB@BN nanocomposites liberated H₂ at 40 °C, and H₂ is pure in the temperature range 40–80 °C, leading to a safe and practical hydrogen storage composite material. Full article

(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)

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