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Inorganics, Volume 2, Issue 3 (September 2014), Pages 377-539

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Editorial

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Open AccessEditorial Frontiers of Energy Storage and Conversion
Inorganics 2014, 2(3), 537-539; doi:10.3390/inorganics2030537
Received: 15 September 2014 / Revised: 20 September 2014 / Accepted: 22 September 2014 / Published: 25 September 2014
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Abstract
This special issue of Inorganics features a Forum for novel materials and approaches for electrochemical energy storage and conversion. Diminishing non-renewable fossil fuels and the resulting unattainability of environment have made us search new sustainable energy resources and develop technology for efficient [...] Read more.
This special issue of Inorganics features a Forum for novel materials and approaches for electrochemical energy storage and conversion. Diminishing non-renewable fossil fuels and the resulting unattainability of environment have made us search new sustainable energy resources and develop technology for efficient utilization of such resources. Green energy sources, such as solar, hydroelectric, thermal and wind energy are partially replacing fossil fuels as means to generate power. Inorganic (solid state) materials are key in the development of advanced devices for the efficient storage and conversion of energy. The grand challenge facing the inorganic chemist is to discover, design rationally and utilize advanced technological materials made from earth-abound elements for these energy storage and conversion processes. Recent spectacular progress in inorganic materials synthesis, characterization, and computational screening has greatly advanced this field, which drove us to edit this issue to provide a window to view the development of this field for the community. This special issue comprises research articles, which highlights some of the most recent advances in new materials for energy storage and conversion. [...] Full article
(This article belongs to the Special Issue Energy Storage and Conversion)

Research

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Open AccessArticle Microstructural Study of IF-WS2 Failure Modes
Inorganics 2014, 2(3), 377-395; doi:10.3390/inorganics2030377
Received: 27 March 2014 / Revised: 3 June 2014 / Accepted: 4 June 2014 / Published: 4 July 2014
Cited by 5 | PDF Full-text (6301 KB) | HTML Full-text | XML Full-text | Supplementary Files
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 [...] Read more.
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
Open AccessArticle Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling
Inorganics 2014, 2(3), 410-423; doi:10.3390/inorganics2030410
Received: 8 May 2014 / Revised: 2 July 2014 / Accepted: 14 July 2014 / Published: 4 August 2014
Cited by 1 | PDF Full-text (2197 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is [...] Read more.
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of great benefit to realize two goals in one step: size reduction and, simultaneously, surface functionalization. A top-down approach for the synthesis of metal oxide particles with in situ surface functionalization is used to modify titania with long alkyl chain organophosphorus coupling agents. A high energy planetary ball mill was used to perform reactive milling using titania as inorganic pigment and long alkyl chain organophosphorus coupling agents like dodecyl and octadecyl phosphonic acid. The final products were characterized by IR, NMR and X-ray fluorescence spectroscopy, thermal and elemental analysis as well as by X-ray powder diffraction and scanning electron microscopy. The process entailed a tribochemical phase transformation from the starting material anatase to a high-pressure modification of titania and the thermodynamically more stable rutile depending on the process parameters. Furthermore, the particles show sizes between 100 nm and 300 nm and a degree of surface coverage up to 0.8 mmol phosphonate per gram. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis) Print Edition available
Open AccessArticle Gold Thione Complexes
Inorganics 2014, 2(3), 424-432; doi:10.3390/inorganics2030424
Received: 2 June 2014 / Revised: 16 July 2014 / Accepted: 18 July 2014 / Published: 4 August 2014
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Abstract
The reaction of the ligand Et4todit (4,5,6,7-Tetrathiocino-[1,2-b:3,4-b']-diimidazolyl-1,3,8,10-tetraethyl-2,9-dithione) with gold complexes leads to the dinuclear gold(I) complexes [{Au(C6F5)}2(Et4todit)] and [Au(Et4todit)]2(OTf)2, which do not [...] Read more.
The reaction of the ligand Et4todit (4,5,6,7-Tetrathiocino-[1,2-b:3,4-b']-diimidazolyl-1,3,8,10-tetraethyl-2,9-dithione) with gold complexes leads to the dinuclear gold(I) complexes [{Au(C6F5)}2(Et4todit)] and [Au(Et4todit)]2(OTf)2, which do not contain any gold-gold interactions, or to the gold(III) derivative [{Au(C6F5)3}2(Et4todit)]. The crystal structures have been established by X-ray diffraction studies and show that the gold centers coordinate to the sulfur atoms of the imidazoline-2-thione groups. Full article
(This article belongs to the Special Issue Frontiers in Gold Chemistry)
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Open AccessArticle Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes
Inorganics 2014, 2(3), 455-467; doi:10.3390/inorganics2030455
Received: 12 May 2014 / Revised: 16 July 2014 / Accepted: 17 July 2014 / Published: 11 August 2014
Cited by 4 | PDF Full-text (5406 KB) | HTML Full-text | XML Full-text | Supplementary Files
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 [...] Read more.
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
Open AccessArticle Half-Lantern Pt(II) and Pt(III) Complexes. New Cyclometalated Platinum Derivatives
Inorganics 2014, 2(3), 508-523; doi:10.3390/inorganics2030508
Received: 7 July 2014 / Revised: 4 August 2014 / Accepted: 5 August 2014 / Published: 26 August 2014
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Abstract
The divalent complex [{Pt(bzq)(μ-L)}2] (1) [Hbzq = benzo[h]quinolone, HL = CF3C4H2N2SH: 4-(trifluoromethyl)pyrimidine-2-thiol] was obtained from equimolar amounts of [Pt(bzq)(NCMe)2]ClO4 and 4-(trifluoromethyl)pyrimidine-2-thiol with an excess [...] Read more.
The divalent complex [{Pt(bzq)(μ-L)}2] (1) [Hbzq = benzo[h]quinolone, HL = CF3C4H2N2SH: 4-(trifluoromethyl)pyrimidine-2-thiol] was obtained from equimolar amounts of [Pt(bzq)(NCMe)2]ClO4 and 4-(trifluoromethyl)pyrimidine-2-thiol with an excess of NEt3. The presence of a low intensity absorption band at 486 nm (CH2Cl2), assignable to a metal-metal-to-ligand charge transfer transition (1MMLCT) [dσ*(Pt)2→π*(bzq)], is indicative of the existence of two platinum centers located in close proximity because the rigidity of the half-lantern structure allows the preservation of these interactions in solution. Compound 1 undergoes two-electron oxidation upon treatment with halogens X2 (X2: Cl2, Br2 or I2) to give the corresponding dihalodiplatinum (III) complexes [{Pt(bzq)(μ-L)X}2] (L = CF3C4H2N2S-κN,S; X: Cl 2, Br 3, I 4). Complexes 24 were also obtained by reaction of 1 with HX (molar ratio 1:2, 10% excess of HX) in THF with yields of about 80% and compound 2 was also obtained by reaction of [{Pt(bzq)(μ-Cl)}2] with HL (4-(trifluoromethyl)pyrimidine-2-thiol) in molar ratio 1:2 in THF, although in small yield. The X-ray structures of 2 and 3 confirmed the half-lantern structure and the anti configuration of the molecules. Both of them show Pt–Pt distances (2.61188(15) Å 2, 2.61767(16) Å 3) in the low range of those observed in Pt2(III,III)X2 half-lantern complexes. Full article
(This article belongs to the Special Issue Organoplatinum Complexes)
Open AccessArticle Synthesis of Ru2Br(μ-O2CC6H4R)4 (R = o-Me, m-Me, p-Me) Using Microwave Activation: Structural and Magnetic Properties
Inorganics 2014, 2(3), 524-536; doi:10.3390/inorganics2030524
Received: 4 July 2014 / Revised: 8 August 2014 / Accepted: 20 August 2014 / Published: 3 September 2014
Cited by 2 | PDF Full-text (3102 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
New bromidotetracarboxylatodiruthenium(II,III) compounds of the type [Ru2Br(μ-O2CC6H4R)4]n [R = o-Me (1), m-Me (2), p-Me (3)] have been prepared using [...] Read more.
New bromidotetracarboxylatodiruthenium(II,III) compounds of the type [Ru2Br(μ-O2CC6H4R)4]n [R = o-Me (1), m-Me (2), p-Me (3)] have been prepared using microwave-assisted methods. Syntheses by means of solvothermal and conventional activations have also been carried out to compare different preparation methods. The crystal structure determination of complexes 13 is also described. All compounds display a typical carboxylate-bridged paddlewheel-type structure with the metal atoms connected by four bridging carboxylate ligands. The axial bromide ligands connect the dimetallic units giving one-dimensional zigzag chains. The magnetic properties of all compounds have also been analyzed. Weak antiferromagnetic intermolecular interactions mediated by the bromide ligands and an appreciable zero field splitting are calculated in the fits of the magnetic data of these complexes. Full article
(This article belongs to the Special Issue Inorganic Syntheses Assisted by Microwave Heating)
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Review

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Open AccessReview Nanostructured Boron Nitride: From Molecular Design to Hydrogen Storage Application
Inorganics 2014, 2(3), 396-409; doi:10.3390/inorganics2030396
Received: 30 April 2014 / Revised: 11 July 2014 / Accepted: 11 July 2014 / Published: 31 July 2014
Cited by 6 | PDF Full-text (8608 KB) | HTML Full-text | XML Full-text
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 [...] Read more.
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
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Open AccessReview Gold Liquid Crystals in the XXI Century
Inorganics 2014, 2(3), 433-454; doi:10.3390/inorganics2030433
Received: 10 June 2014 / Revised: 16 July 2014 / Accepted: 17 July 2014 / Published: 6 August 2014
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Abstract
Since the first gold liquid crystal was described in 1986, much effort has been done to prepare new compounds bearing this property. The review deals with the last results obtained in this new century. Gold(I) has a strong affinity to give linear [...] Read more.
Since the first gold liquid crystal was described in 1986, much effort has been done to prepare new compounds bearing this property. The review deals with the last results obtained in this new century. Gold(I) has a strong affinity to give linear co-ordination and metal-metal interactions, which produce a rich supramolecular chemistry, and can promote the behavior as liquid crystal. Therefore, most liquid crystals are based on rod-like gold(I) compounds, while gold(III) liquid crystals are scarce. Calamitic and discotic mesogens have been reported, as well as chiral liquid crystals. Weak interactions such as H-bonds have also been used to obtain gold mesogens. Some of them exhibit additional properties, such as color, luminescence, and chirality. Luminescence has been reported, not only in the solid state or in solution, but also in the mesophase. This is relevant for applications in LEDs (Light Emitting Diodes), information storage, and sensors. Full article
(This article belongs to the Special Issue Frontiers in Gold Chemistry)
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Open AccessReview Microwave Plasma Synthesis of Materials—From Physics and Chemistry to Nanoparticles: A Materials Scientist’s Viewpoint
Inorganics 2014, 2(3), 468-507; doi:10.3390/inorganics2030468
Received: 10 June 2014 / Revised: 6 August 2014 / Accepted: 11 August 2014 / Published: 18 August 2014
Cited by 7 | PDF Full-text (5180 KB) | HTML Full-text | XML Full-text
Abstract
In this review, microwave plasma gas-phase synthesis of inorganic materials and material groups is discussed from the application-oriented perspective of a materials scientist: why and how microwave plasmas are applied for the synthesis of materials? First, key players in this research field [...] Read more.
In this review, microwave plasma gas-phase synthesis of inorganic materials and material groups is discussed from the application-oriented perspective of a materials scientist: why and how microwave plasmas are applied for the synthesis of materials? First, key players in this research field will be identified, and a brief overview on publication history on this topic is given. The fundamental basics, necessary to understand the processes ongoing in particle synthesis—one of the main applications of microwave plasma processes—and the influence of the relevant experimental parameters on the resulting particles and their properties will be addressed. The benefit of using microwave plasma instead of conventional gas phase processes with respect to chemical reactivity and crystallite nucleation will be reviewed. The criteria, how to choose an appropriate precursor to synthesize a specific material with an intended application is discussed. A tabular overview on all type of materials synthesized in microwave plasmas and other plasma methods will be given, including relevant citations. Finally, property examples of three groups of nanomaterials synthesized with microwave plasma methods, bare Fe2O3 nanoparticles, different core/shell ceramic/organic shell nanoparticles, and Sn-based nanocomposites, will be described exemplarily, comprising perspectives of applications. Full article
(This article belongs to the Special Issue Inorganic Syntheses Assisted by Microwave Heating)

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