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Inorganics, Volume 2, Issue 2 (June 2014), Pages 155-376

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Research

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Open AccessArticle Electromechanical Properties of Small Transition-Metal Dichalcogenide Nanotubes
Inorganics 2014, 2(2), 155-167; doi:10.3390/inorganics2020155
Received: 14 March 2014 / Revised: 11 April 2014 / Accepted: 11 April 2014 / Published: 23 April 2014
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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 [...] Read more.
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
Open AccessCommunication Qualifying the Role of Indium in the Multiple-Filled Ce0.1InxYb0.2Co4Sb12 Skutterudite
Inorganics 2014, 2(2), 168-176; doi:10.3390/inorganics2020168
Received: 13 February 2014 / Revised: 8 April 2014 / Accepted: 14 April 2014 / Published: 29 April 2014
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Abstract
Literature confirms an improvement in the overall TE properties due to the in situ InSb nano-dispersed phases located along the grain boundaries in several double-filled InxYzCo4Sb12 skutterudites. However, the single-filled InxCo4Sb [...] Read more.
Literature confirms an improvement in the overall TE properties due to the in situ InSb nano-dispersed phases located along the grain boundaries in several double-filled InxYzCo4Sb12 skutterudites. However, the single-filled InxCo4Sb12 reports contribute enhancement in TE properties solely on the nature of In as a void filler. To qualify the effect of In on the TE properties on multiple-filled skutterudites several multiple-filled Ce0.1InxYb0.2Co4Sb12 skutterudite samples, with nominal composition Ce0.1InyYb0.2Co4Sb12 (0 ≤ y ≤ 0.2), were synthesized. A double-filled base-line sample Ce0.1Yb0.2Co4Sb12 was also synthesized and characterized to create a much fuller depiction of the nature of In and its impact on the TE properties of the filled Co4Sb12-based skutterudite materials. Our results confirm that small amounts of In can be effective at increasing electrical conductivity in the multiple-filled Ce0.1InyYb0.2Co4Sb12 skutterudite. An increased mobility and thus electrical conductivity result in a 15% increase in the dimensionless Figure of Merit, ZT, in the nominal sample composition, Ce0.1In0.05Yb0.2Co4Sb12, which exhibits a state of the art ZT > 1.4 at T = 820 K. Full article
(This article belongs to the Special Issue Energy Storage and Conversion)
Open AccessArticle Single- to Triple-Wall WS2 Nanotubes Obtained by High-Power Plasma Ablation of WS2 Multiwall Nanotubes
Inorganics 2014, 2(2), 177-190; doi:10.3390/inorganics2020177
Received: 15 March 2014 / Revised: 21 April 2014 / Accepted: 21 April 2014 / Published: 29 April 2014
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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 [...] Read more.
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, WS2 nanotubes 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
Open AccessArticle IF-WS2/Nanostructured Carbon Hybrids Generation and Their Characterization
Inorganics 2014, 2(2), 211-232; doi:10.3390/inorganics2020211
Received: 5 March 2014 / Revised: 24 April 2014 / Accepted: 28 April 2014 / Published: 9 May 2014
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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 WS [...] Read more.
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-WS2 and G/IF-WS2 were 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-WS2 and G/IF-WS2 products 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-WS2 and G/IF-WS2 hybrids 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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Open AccessArticle Supercritical Fluid Synthesis of LiCoPO4 Nanoparticles and Their Application to Lithium Ion Battery
Inorganics 2014, 2(2), 233-247; doi:10.3390/inorganics2020233
Received: 31 October 2013 / Revised: 23 January 2014 / Accepted: 19 May 2014 / Published: 28 May 2014
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Abstract
In this work, LiCoPO4 nanoparticles were synthesized by supercritical fluid method using cobalt nitrate hexahydrate (Co(NO3)2 6H2O) and cobalt acetate tetrahydrate (C4H6CoO4 4H2O) as starting materials. The effect of [...] Read more.
In this work, LiCoPO4 nanoparticles were synthesized by supercritical fluid method using cobalt nitrate hexahydrate (Co(NO3)2 6H2O) and cobalt acetate tetrahydrate (C4H6CoO4 4H2O) as starting materials. The effect of starting materials on particle morphology, size, and the crystalline phase were investigated. The as-synthesized samples were systematically characterized by XRD, TEM, STEM, EDS, BET, and TG and charge-discharge measurements. In addition, Rietveld refinement analysis was performed. The electrochemical measurements of LiCoPO4 nanoparticles have shown differences in capacities depending on the starting materials used in the synthesis and the results have been discussed in this paper. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis) Print Edition available
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Open AccessArticle From Stable ZnO and GaN Clusters to Novel Double Bubbles and Frameworks
Inorganics 2014, 2(2), 248-263; doi:10.3390/inorganics2020248
Received: 1 April 2014 / Revised: 4 May 2014 / Accepted: 5 May 2014 / Published: 28 May 2014
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Abstract
A bottom up approach is employed in the design of novel materials: first, gas-phase “double bubble” clusters are constructed from high symmetry, Th, 24 and 96 atom, single bubbles of ZnO and GaN. These are used to construct bulk frameworks. [...] Read more.
A bottom up approach is employed in the design of novel materials: first, gas-phase “double bubble” clusters are constructed from high symmetry, Th, 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
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Open AccessArticle Microwave-Assisted Synthesis of Boron-Modified TiO2 Nanocrystals
Inorganics 2014, 2(2), 264-277; doi:10.3390/inorganics2020264
Received: 4 April 2014 / Revised: 19 May 2014 / Accepted: 21 May 2014 / Published: 6 June 2014
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Abstract
An efficient microwave-assisted synthesis of TiO2:(B) nanorods, using titanium tetraisopropoxide (TTIP), benzyl alcohol as the solvent, together with boric acid and oleic acid as the additive reagents, has been developed. Chemical modification of TTIP by oleic acid was demonstrated as [...] Read more.
An efficient microwave-assisted synthesis of TiO2:(B) nanorods, using titanium tetraisopropoxide (TTIP), benzyl alcohol as the solvent, together with boric acid and oleic acid as the additive reagents, has been developed. Chemical modification of TTIP by oleic acid was demonstrated as a rational strategy to tune the shape of TiO2 nanocrystals toward nanorod formation. The differently-shaped TiO2:(B) nanocrystals were characterized in detail by transmission electron microscopy (TEM), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and nitrogen absorption-desorption. Oleic acid coordinated on the nanocrystal surface was removed by the reduction of its carboxyl group, and the photocatalytic activity of bare TiO2 nanocrystals, under visible light irradiation, was also evaluated. The synthesized TiO2 anatase nanorods exhibited a good photoactivity and completely degraded Rhodamine B solution within three hours. Full article
(This article belongs to the Special Issue Inorganic Syntheses Assisted by Microwave Heating)
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Open AccessArticle Microwave Plasma Production of Metal Nanopowders
Inorganics 2014, 2(2), 278-290; doi:10.3390/inorganics2020278
Received: 27 February 2014 / Revised: 23 May 2014 / Accepted: 5 June 2014 / Published: 12 June 2014
Cited by 2 | PDF Full-text (3849 KB) | HTML Full-text | XML Full-text
Abstract
Metal and metal alloy nanopowders were prepared by using the microwave plasma synthesis method. The microwave plasma was operated in atmospheric pressure at a frequency of 2.45 GHz. The precursor decomposed thermally in the plasma reaction region and the products were then [...] Read more.
Metal and metal alloy nanopowders were prepared by using the microwave plasma synthesis method. The microwave plasma was operated in atmospheric pressure at a frequency of 2.45 GHz. The precursor decomposed thermally in the plasma reaction region and the products were then condensed in the heat exchanger, were separated from the gas by the powder filter, and then finally collected in the powder collector. The effect of various processing parameters such as plasma gas, carrier gas, cooling gas, precursor raw materials and feeding rate were studied in this work. Cu, Mo, W, Mo-Ni and Fe-Co nanopowders were successfully prepared by using the microwave plasma synthesis method. The processing conditions can be tuned to manipulate the particle size of the nanopowders. Full article
(This article belongs to the Special Issue Inorganic Syntheses Assisted by Microwave Heating)
Open AccessArticle Thermoplastic Polymer Nanocomposites Based on Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes
Inorganics 2014, 2(2), 291-312; doi:10.3390/inorganics2020291
Received: 3 March 2014 / Revised: 3 June 2014 / Accepted: 5 June 2014 / Published: 12 June 2014
Cited by 12 | PDF Full-text (1843 KB) | HTML Full-text | XML Full-text
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 [...] Read more.
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
Open AccessArticle Continuous Production of IF-WS2 Nanoparticles by a Rotary Process
Inorganics 2014, 2(2), 313-333; doi:10.3390/inorganics2020313
Received: 14 March 2014 / Revised: 6 May 2014 / Accepted: 4 June 2014 / Published: 13 June 2014
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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 [...] Read more.
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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Open AccessArticle Gas-Phase and Microsolvated Glycine Interacting with Boron Nitride Nanotubes. A B3LYP-D2* Periodic Study
Inorganics 2014, 2(2), 334-350; doi:10.3390/inorganics2020334
Received: 9 May 2014 / Revised: 29 May 2014 / Accepted: 30 May 2014 / Published: 18 June 2014
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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 [...] Read more.
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
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Open AccessArticle Thermoelectric Properties of Mg2Si Produced by New Chemical Route and SPS
Inorganics 2014, 2(2), 351-362; doi:10.3390/inorganics2020351
Received: 15 January 2014 / Revised: 9 May 2014 / Accepted: 27 May 2014 / Published: 20 June 2014
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Abstract
This paper reports about a new synthesis method for preparing Mg2Si in an efficient way. The intermetallic Mg2Si-phase forms gradually from a mixture of Mg and Si fine powder during exposure to hydrogen atmosphere, which reacts in a [...] Read more.
This paper reports about a new synthesis method for preparing Mg2Si in an efficient way. The intermetallic Mg2Si-phase forms gradually from a mixture of Mg and Si fine powder during exposure to hydrogen atmosphere, which reacts in a vacuum vessel at 350 °C. The resulting powder has the same particle size (100 µm) compared with commercial Mg2Si powder, but higher reactivity due to large surface area from particulate morphology. Both types of powders were compacted by spark plasma sintering (SPS) experiments at 627, 602, 597, and 400 °C for 600 s with a compaction pressure of 80 MPa. The thermoelectric characterization was performed with low and high temperature gradients of ΔT = 10 K up to 600 K. The results confirmed a Seebeck coefficient of −0.14 mV/K for specimens sintered from both powders. The small difference in total performance between purchased and produced power is considered to be due to the effect of impurities. The best values were obtained for n-type Mg2Si doped with 3% Bi yielding a Seebeck coefficient of −0.2 mV/K, ZT = 0.45) and electric output power of more than 6 µW. Full article
(This article belongs to the Special Issue Energy Storage and Conversion)
Open AccessArticle The Role of Lead (Pb) in the High Temperature Formation of MoS2 Nanotubes
Inorganics 2014, 2(2), 363-376; doi:10.3390/inorganics2020363
Received: 23 April 2014 / Revised: 27 May 2014 / Accepted: 4 June 2014 / Published: 23 June 2014
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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 [...] Read more.
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 (PbMo) leads to p-type semiconducting character; while intercalation of MoS2 by Pb atoms (Pby/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
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Review

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Open AccessReview Direct Energy Supply to the Reaction Mixture during Microwave-Assisted Hydrothermal and Combustion Synthesis of Inorganic Materials
Inorganics 2014, 2(2), 191-210; doi:10.3390/inorganics2020191
Received: 22 November 2013 / Revised: 23 January 2014 / Accepted: 28 April 2014 / Published: 5 May 2014
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Abstract
The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW) radiation into heat is useful in overcoming the activation energy barriers associated [...] Read more.
The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW) radiation into heat is useful in overcoming the activation energy barriers associated with chemical transformations, but the use of microwaves can be further extended to higher temperatures, thus creating unusual high-energy environments. In devising synthetic methodologies to engineered nanomaterials, hydrothermal synthesis and solution combustion synthesis can be used as reference systems to illustrate effects related to microwave irradiation. In the first case, energy is transferred to the entire reaction volume, causing a homogeneous temperature rise within a closed vessel in a few minutes, hence assuring uniform crystal growth at the nanometer scale. In the second case, strong exothermic combustion syntheses can benefit from the application of microwaves to convey energy to the reaction not only during the ignition step, but also while it is occurring and even after its completion. In both approaches, however, the direct interaction of microwaves with the reaction mixture can lead to practically gradient-less heating profiles, on the basis of which the main observed characteristics and properties of the aforementioned reactions and products can be explained. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis) Print Edition available

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