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Materials, Volume 10, Issue 3 (March 2017)

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Cover Story (view full-size image) From diapers to agricultural use, from drug release to self-healing concrete, superabsorbent [...] Read more.
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Open AccessArticle Study of the Corrosion Resistance of Austenitic Stainless Steels during Conversion of Waste to Biofuel
Materials 2017, 10(3), 325; https://doi.org/10.3390/ma10030325
Received: 1 February 2017 / Revised: 14 March 2017 / Accepted: 15 March 2017 / Published: 22 March 2017
Cited by 1 | PDF Full-text (4901 KB) | HTML Full-text | XML Full-text
Abstract
The paper deals with the corrosion behavior of stainless steels as candidate materials for biofuel production plants by liquefaction process of the sorted organic fraction of municipal solid waste. Corrosion tests were carried out on AISI 316L and AISI 304L stainless steels at
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The paper deals with the corrosion behavior of stainless steels as candidate materials for biofuel production plants by liquefaction process of the sorted organic fraction of municipal solid waste. Corrosion tests were carried out on AISI 316L and AISI 304L stainless steels at 250 °C in a batch reactor during conversion of raw material to bio-oil (biofuel precursor), by exposing specimens either to water/oil phase or humid gas phase. General corrosion rate was measured by weight loss tests. The susceptibility to stress corrosion cracking was evaluated by means of U-bend specimens and slow stress rate tests at 10−6 or 10−5 s−1 strain rate. After tests, scanning electron microscope analysis was carried out to detect cracks and localized attacks. The results are discussed in relation with exposure conditions. They show very low corrosion rates strictly dependent upon time and temperature. No stress corrosion cracking was observed on U-bend specimens, under constant loading. Small cracks confined in the necking cone of specimens prove that stress corrosion cracking only occurred during slow strain rate tests at stresses exceeding the yield strength. Full article
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Open AccessArticle Development of AlN and TiB2 Composites with Nb2O5, Y2O3 and ZrO2 as Sintering Aids
Materials 2017, 10(3), 324; https://doi.org/10.3390/ma10030324
Received: 19 December 2016 / Revised: 8 March 2017 / Accepted: 13 March 2017 / Published: 22 March 2017
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Abstract
The synthesis of AlN and TiB2 by spark plasma sintering (SPS) and the effect of Nb2O5, Y2O3 and ZrO2 additions on the mechanical properties and densification of the produced composites is reported and discussed.
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The synthesis of AlN and TiB2 by spark plasma sintering (SPS) and the effect of Nb2O5, Y2O3 and ZrO2 additions on the mechanical properties and densification of the produced composites is reported and discussed. After the SPS process, dense AlN and TiB2 composites with Nb2O5, Y2O3 and ZrO2 were successfully prepared. X-ray diffraction analysis showed that in the AlN composites, the addition of Nb2O5 gives rise to Nb4N3 during sintering. The compound Y3Al5O12 (YAG) was observed as precipitate in the sample with Y2O3. X-ray diffraction analysis of the TiB2 composites showed TiB2 as a single phase in these materials. The maximum Vickers and toughness values were 14.19 ± 1.43 GPa and 27.52 ± 1.75 GPa for the AlN and TiB2 composites, respectively. Full article
(This article belongs to the Section Advanced Composites)
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Open AccessArticle Integration of Electrodeposited Ni-Fe in MEMS with Low-Temperature Deposition and Etch Processes
Materials 2017, 10(3), 323; https://doi.org/10.3390/ma10030323
Received: 9 February 2017 / Revised: 12 March 2017 / Accepted: 17 March 2017 / Published: 22 March 2017
Cited by 1 | PDF Full-text (41645 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
This article presents a set of low-temperature deposition and etching processes for the integration of electrochemically deposited Ni-Fe alloys in complex magnetic microelectromechanical systems, as Ni-Fe is known to suffer from detrimental stress development when subjected to excessive thermal loads. A selective etch
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This article presents a set of low-temperature deposition and etching processes for the integration of electrochemically deposited Ni-Fe alloys in complex magnetic microelectromechanical systems, as Ni-Fe is known to suffer from detrimental stress development when subjected to excessive thermal loads. A selective etch process is reported which enables the copper seed layer used for electrodeposition to be removed while preserving the integrity of Ni-Fe. In addition, a low temperature deposition and surface micromachining process is presented in which silicon dioxide and silicon nitride are used, respectively, as sacrificial material and structural dielectric. The sacrificial layer can be patterned and removed by wet buffered oxide etch or vapour HF etching. The reported methods limit the thermal budget and minimise the stress development in Ni-Fe. This combination of techniques represents an advance towards the reliable integration of Ni-Fe components in complex surface micromachined magnetic MEMS. Full article
(This article belongs to the Section Manufacturing Processes and Systems)
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Open AccessArticle Enhanced Unipolar Resistive Switching Characteristics of Hf0.5Zr0.5O2 Thin Films with High ON/OFF Ratio
Materials 2017, 10(3), 322; https://doi.org/10.3390/ma10030322
Received: 16 January 2017 / Revised: 3 March 2017 / Accepted: 13 March 2017 / Published: 22 March 2017
Cited by 3 | PDF Full-text (1743 KB) | HTML Full-text | XML Full-text
Abstract
A metal–insulator–metal structure resistive switching device based on H0.5Z0.5O2 (HZO) thin film deposited by pulse laser deposition (PLD) has been investigated for resistive random access memory (RRAM) applications. The devices demonstrated bistable and reproducible unipolar resistive switching (RS)
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A metal–insulator–metal structure resistive switching device based on H0.5Z0.5O2 (HZO) thin film deposited by pulse laser deposition (PLD) has been investigated for resistive random access memory (RRAM) applications. The devices demonstrated bistable and reproducible unipolar resistive switching (RS) behaviors with an extremely high OFF/ON ratio over 5400. The retention property had no degradation at 6 × 104 s. The current–voltage characteristics of the HZO samples showed a Schottky emission conduction in the high voltage region (Vreset < V < Vset), while at the low voltage region (V < Vreset), the ohmic contact and space charge limited conduction (SCLC) are suggested to be responsible for the low and high resistance states, respectively. Combined with the conductance mechanism, the RS behaviors are attributed to joule heating and redox reactions in the HZO thin film induced by the external electron injection. Full article
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Open AccessArticle 3D Molding of Veneers by Mechanical and Pneumatic Methods
Materials 2017, 10(3), 321; https://doi.org/10.3390/ma10030321
Received: 19 November 2016 / Revised: 9 March 2017 / Accepted: 14 March 2017 / Published: 22 March 2017
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Abstract
This paper deals with the influence of selected methods (mechanical and pneumatic) as well as various factors (wood species, moisture content, veneer shape, punch diameter, laminating foil thickness, holding method, plasticizing) on 3D molding of veneers. 3D molding was evaluated on the basis
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This paper deals with the influence of selected methods (mechanical and pneumatic) as well as various factors (wood species, moisture content, veneer shape, punch diameter, laminating foil thickness, holding method, plasticizing) on 3D molding of veneers. 3D molding was evaluated on the basis of maximum deflection of birch and beech veneers. Cracks and warping edges were also evaluated in selected groups of mechanical molding. Mechanical methods tested veneers with various treatments (steaming, water and ammonia plasticizing and lamination). The pneumatic method was based on veneer shaping using air pressure. The results indicate that birch veneers are more suitable for 3D molding. The differences between the mechanical and pneumatic methods were not considerable. The most suitable method for mechanical 3D molding was the veneer lamination by polyethylene foils with thicknesses of 80 and 125 μm, inasmuch as these achieved better results than veneer plasticized by steam. The occurrence of cracks was more frequent in beech veneers, whereas, edge warping occurred at similar rates for both wood species and depends rather on holding method during 3D molding. Use of the ammonia solution is more suitable and there occurs no marked increase in moisture as happens when soaking in water. Full article
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Open AccessArticle The Effect of Thickness of Resorbable Bacterial Cellulose Membrane on Guided Bone Regeneration
Materials 2017, 10(3), 320; https://doi.org/10.3390/ma10030320
Received: 13 February 2017 / Revised: 14 March 2017 / Accepted: 17 March 2017 / Published: 21 March 2017
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Abstract
This study introduces the effect of the thickness of a bacterial cellulose membrane by comparing the bone regeneration effect on rat skulls when using a collagen membrane and different thicknesses of resorbable bacterial cellulose membranes for guided bone regeneration. Barrier membranes of 0.10
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This study introduces the effect of the thickness of a bacterial cellulose membrane by comparing the bone regeneration effect on rat skulls when using a collagen membrane and different thicknesses of resorbable bacterial cellulose membranes for guided bone regeneration. Barrier membranes of 0.10 mm, 0.15 mm, and 0.20 mm in thickness were made using bacterial cellulose produced as microbial fermentation metabolites. Mechanical strength was investigated, and new bone formation was evaluated through animal experimental studies. Experimental animals were sacrificed after having 2 weeks and 8 weeks of recovery, and specimens were processed for histologic and histomorphometric analyses measuring the area of bone regeneration (%) using an image analysis program. In 2 weeks, bone-like materials and fibrous connective tissues were observed in histologic analysis. In 8 weeks, all experimental groups showed the arrangement of osteoblasts surrounding the supporting body on the margin and center of the bone defect region. However, the amount of new bone formation was significantly higher (p < 0.05) in bacterial cellulose membrane with 0.10 mm in thickness compared to the other experimental groups. Within the limitations of this study, a bacterial cellulose membrane with 0.10 mm thickness induced the most effective bone regeneration. Full article
(This article belongs to the Section Biomaterials)
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Open AccessCommunication High Performance Complementary Circuits Based on p-SnO and n-IGZO Thin-Film Transistors
Materials 2017, 10(3), 319; https://doi.org/10.3390/ma10030319
Received: 5 January 2017 / Revised: 28 February 2017 / Accepted: 15 March 2017 / Published: 21 March 2017
Cited by 5 | PDF Full-text (1569 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Oxide semiconductors are regarded as promising materials for large-area and/or flexible electronics. In this work, a ring oscillator based on n-type indium-gallium-zinc-oxide (IGZO) and p-type tin monoxide (SnO) is presented. The IGZO thin-film transistor (TFT) shows a linear mobility of
[...] Read more.
Oxide semiconductors are regarded as promising materials for large-area and/or flexible electronics. In this work, a ring oscillator based on n-type indium-gallium-zinc-oxide (IGZO) and p-type tin monoxide (SnO) is presented. The IGZO thin-film transistor (TFT) shows a linear mobility of 11.9 cm2/(V∙s) and a threshold voltage of 12.2 V. The SnO TFT exhibits a mobility of 0.51 cm2/(V∙s) and a threshold voltage of 20.1 V which is suitable for use with IGZO TFTs to form complementary circuits. At a supply voltage of 40 V, the complementary inverter shows a full output voltage swing and a gain of 24 with both TFTs having the same channel length/channel width ratio. The three-stage ring oscillator based on IGZO and SnO is able to operate at 2.63 kHz and the peak-to-peak oscillation amplitude reaches 36.1 V at a supply voltage of 40 V. The oxide-based complementary circuits, after further optimization of the operation voltage, may have wide applications in practical large-area flexible electronics. Full article
(This article belongs to the Special Issue Oxide Semiconductor Thin-Film Transistor)
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Open AccessArticle Hot Deformation and Processing Window Optimization of a 70MnSiCrMo Carbide-Free Bainitic Steel
Materials 2017, 10(3), 318; https://doi.org/10.3390/ma10030318
Received: 24 January 2017 / Revised: 8 March 2017 / Accepted: 15 March 2017 / Published: 21 March 2017
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Abstract
The hot deformation behavior of a high carbon carbide-free bainitic steel was studied through isothermal compression tests that were performed on a Gleeble-1500D thermal mechanical simulator at temperatures of 1223–1423 K and strain rates of 0.01–5 s−1. The flow behavior, constitutive
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The hot deformation behavior of a high carbon carbide-free bainitic steel was studied through isothermal compression tests that were performed on a Gleeble-1500D thermal mechanical simulator at temperatures of 1223–1423 K and strain rates of 0.01–5 s−1. The flow behavior, constitutive equations, dynamic recrystallization (DRX) characteristics, and processing map were respectively analyzed in detail. It is found that the flow stress increases with increasing the strain rate and decreases with increasing the temperature, and the single-peak DRX can be easily observed at high temperatures and/or low strain rates. The internal relationship between the flow stress and processing parameters was built by the constitutive equations embracing a parameter of Z/A, where the activation energy for hot deformation is 351.539 kJ/mol and the stress exponent is 4.233. In addition, the DRX evolution and the critical conditions for starting DRX were discussed. Then the model of the DRX volume fraction was developed with satisfied predictability. Finally, the processing maps at different strains were constructed according to the dynamic material model. The safety domains and flow instability regions were identified. The best processing parameters of this steel are within the temperature range of 1323–1423 K and strain rate range of 0.06–1 s−1. Full article
(This article belongs to the Section Manufacturing Processes and Systems)
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Open AccessArticle Towards Highly Performing and Stable PtNi Catalysts in Polymer Electrolyte Fuel Cells for Automotive Application
Materials 2017, 10(3), 317; https://doi.org/10.3390/ma10030317
Received: 28 December 2016 / Revised: 13 March 2017 / Accepted: 15 March 2017 / Published: 21 March 2017
Cited by 5 | PDF Full-text (6692 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
In order to help the introduction on the automotive market of polymer electrolyte fuel cells (PEFCs), it is mandatory to develop highly performing and stable catalysts. The main objective of this work is to investigate PtNi/C catalysts in a PEFC under low relative
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In order to help the introduction on the automotive market of polymer electrolyte fuel cells (PEFCs), it is mandatory to develop highly performing and stable catalysts. The main objective of this work is to investigate PtNi/C catalysts in a PEFC under low relative humidity and pressure conditions, more representative of automotive applications. Carbon supported PtNi nanoparticles were prepared by reduction of metal precursors with formic acid and successive thermal and leaching treatments. The effect of the chemical composition, structure and surface characteristics of the synthesized samples on their electrochemical behavior was investigated. The catalyst characterized by a larger Pt content (Pt3Ni2/C) presented the highest catalytic activity (lower potential losses in the activation region) among the synthesized bimetallic PtNi catalysts and the commercial Pt/C, used as the reference material, after testing at high temperature (95 °C) and low humidification (50%) conditions for automotive applications, showing a cell potential (ohmic drop-free) of 0.82 V at 500 mA·cm−2. In order to assess the electro-catalysts stability, accelerated degradation tests were carried out by cycling the cell potential between 0.6 V and 1.2 V. By comparing the electrochemical and physico-chemical parameters at the beginning of life (BoL) and end of life (EoL), it was demonstrated that the Pt1Ni1/C catalyst was the most stable among the catalyst series, with only a 2% loss of voltage at 200 mA·cm−2 and 12.5% at 950 mA·cm−2. However, further improvements are needed to produce durable catalysts. Full article
(This article belongs to the Special Issue Advanced Materials in Polymer Electrolyte Fuel Cells)
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Open AccessArticle Negative Temperature Dependence of Recrystallized Grain Size: Formulation and Experimental Confirmation on Copper
Materials 2017, 10(3), 308; https://doi.org/10.3390/ma10030308
Received: 7 December 2016 / Revised: 21 February 2017 / Accepted: 10 March 2017 / Published: 21 March 2017
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Abstract
The catalyzing effect on nucleation of recrystallization from existing grains resulting from previous lower temperature deformation is analyzed, analogous to the size effect of foreign nucleus in heterogeneous nucleation. Analytical formulation of the effective nucleation site for recrystallization leads to a negative temperature
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The catalyzing effect on nucleation of recrystallization from existing grains resulting from previous lower temperature deformation is analyzed, analogous to the size effect of foreign nucleus in heterogeneous nucleation. Analytical formulation of the effective nucleation site for recrystallization leads to a negative temperature dependence of recrystallized grain size of metals. Non-isochronal annealing—where annealing time is set just enough for the completion of recrystallization at different temperatures—is conducted on pure copper after severe plastic deformation. More homogeneous and smaller grains are obtained at higher annealing temperature. The good fit between analytical and experimental results unveils the intrinsic feature of this negative temperature dependence of recrystallized grain size. Full article
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Open AccessArticle Experimental Study on the Fire Properties of Nitrocellulose with Different Structures
Materials 2017, 10(3), 316; https://doi.org/10.3390/ma10030316
Received: 5 January 2017 / Revised: 6 March 2017 / Accepted: 16 March 2017 / Published: 20 March 2017
Cited by 3 | PDF Full-text (4959 KB) | HTML Full-text | XML Full-text
Abstract
In order to ensure the safety of inflammable and explosive chemical substance such as nitrocellulose (NC) mixtures in the process of handing, storage, and usage, it is necessary to obtain the fire properties of NC with different exterior structures. In present study, fire
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In order to ensure the safety of inflammable and explosive chemical substance such as nitrocellulose (NC) mixtures in the process of handing, storage, and usage, it is necessary to obtain the fire properties of NC with different exterior structures. In present study, fire properties of two commonly used nitrocelluloses with soft fiber structure and white chip structure were investigated by scanning electron microscope (SEM) and the ISO 5660 cone calorimeter. Experimental findings revealed that the most important fire properties such as ignition time, mass loss rate and ash content exhibited significant differences between the two structures of NC. Compared with the soft fiber NC, chip NC possesses a lower fire hazard, and its heat release rate intensity (HRRI) is mainly affected by the sample mass. In addition, oxygen consumption (OC) calorimetry method was compared with thermal chemistry (TC) method based on stoichiometry for HRRI calculation. HRRI results of NC with two structures obtained by these two methods showed a good consistency. Full article
(This article belongs to the Section Manufacturing Processes and Systems)
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Open AccessArticle Microwave-Assisted Catalytic Synthesis of Bio-Based Copolymers from Waste Cooking Oil
Materials 2017, 10(3), 315; https://doi.org/10.3390/ma10030315
Received: 9 January 2017 / Revised: 10 March 2017 / Accepted: 14 March 2017 / Published: 20 March 2017
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Abstract
Solvent-free copolymerization of epoxides derived from fatty esters of waste cooking oil with phthalic anhydride using (salen)CrIIICl as catalyst and n-Bu4NCl/DMAP (tetrabutylammonium chloride/4-(dimethylamino)pyridine) as co-catalysts was carried out for the first time under microwave irradiation, where reaction time was
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Solvent-free copolymerization of epoxides derived from fatty esters of waste cooking oil with phthalic anhydride using (salen)CrIIICl as catalyst and n-Bu4NCl/DMAP (tetrabutylammonium chloride/4-(dimethylamino)pyridine) as co-catalysts was carried out for the first time under microwave irradiation, where reaction time was reduced from a number of hours to minutes. The polyesters were obtained with molecular weight (Mw = 3100–6750 g/mol) and dispersity values (D = 1.18–1.92) when (salen)CrIIICl/n-Bu4NCl was used as catalysts. Moreover, in the case of DMAP as a co-catalyst, polyesters with improved molecular weight (Mw = 5500–6950 g/mol) and narrow dispersity values (D = 1.07–1.28) were obtained even at reduced concentrations of (salen)CrIIICl and DMAP. The obtained products were characterized and evaluated by attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), proton nuclear magnetic resonance (1H-NMR) spectroscopy, gel permeation chromatography (GPC), thermogravimetric analysis (TGA) and differential scanning calorimetric (DSC) Techniques. Full article
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Open AccessArticle VO2 Thermochromic Films on Quartz Glass Substrate Grown by RF-Plasma-Assisted Oxide Molecular Beam Epitaxy
Materials 2017, 10(3), 314; https://doi.org/10.3390/ma10030314
Received: 21 January 2017 / Revised: 14 March 2017 / Accepted: 15 March 2017 / Published: 19 March 2017
Cited by 1 | PDF Full-text (3165 KB) | HTML Full-text | XML Full-text
Abstract
Vanadium dioxide (VO2) thermochromic thin films with various thicknesses were grown on quartz glass substrates by radio frequency (RF)-plasma assisted oxide molecular beam epitaxy (O-MBE). The crystal structure, morphology and chemical stoichiometry were investigated systemically by X-ray diffraction (XRD), atomic force
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Vanadium dioxide (VO2) thermochromic thin films with various thicknesses were grown on quartz glass substrates by radio frequency (RF)-plasma assisted oxide molecular beam epitaxy (O-MBE). The crystal structure, morphology and chemical stoichiometry were investigated systemically by X-ray diffraction (XRD), atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) analyses. An excellent reversible metal-to-insulator transition (MIT) characteristics accompanied by an abrupt change in both electrical resistivity and optical infrared (IR) transmittance was observed from the optimized sample. Remarkably, the transition temperature (TMIT) deduced from the resistivity-temperature curve was reasonably consistent with that obtained from the temperature-dependent IR transmittance. Based on Raman measurement and XPS analyses, the observations were interpreted in terms of residual stresses and chemical stoichiometry. This achievement will be of great benefit for practical application of VO2-based smart windows. Full article
(This article belongs to the Special Issue Metal-Insulator Transition)
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Open AccessArticle Two 8-Hydroxyquinolinate Based Supramolecular Coordination Compounds: Synthesis, Structures and Spectral Properties
Materials 2017, 10(3), 313; https://doi.org/10.3390/ma10030313
Received: 9 February 2017 / Revised: 3 March 2017 / Accepted: 16 March 2017 / Published: 18 March 2017
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Abstract
Two new Cr(III) complexes based on 2-substituted 8-hydroxyquinoline ligands, namely [Cr(L1)3] (1), (HL1=(E)-2-[2-(4-nitro-phenyl)-vinyl]-8-hydroxy-quinoline) and [Cr(L2)3] (2), (HL2=(E)-2-[2-(4-chloro-phenyl)vinyl]-8-hydroxy-quinoline), were prepared by a facile hydrothermal method and characterized thoroughly
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Two new Cr(III) complexes based on 2-substituted 8-hydroxyquinoline ligands, namely [Cr(L1)3] (1), (HL1=(E)-2-[2-(4-nitro-phenyl)-vinyl]-8-hydroxy-quinoline) and [Cr(L2)3] (2), (HL2=(E)-2-[2-(4-chloro-phenyl)vinyl]-8-hydroxy-quinoline), were prepared by a facile hydrothermal method and characterized thoroughly by single crystal X-ray diffraction, powder X-ray diffraction, FTIR, TGA, ESI-MS, UV-Visible absorption spectra and fluorescence emission spectra. Single crystal X-ray diffraction analyses showed that the two compounds featured 3D supramolecular architectures constructed from noncovalent interactions, such as π···π stacking, C-H···π, C-H···O, C-Cl···π, C-H···Cl interactions. The thermogravimetric analysis and ESI-MS study of compounds 1 and 2 suggested that the Cr(III) complexes possessed good stability both in solid and solution. In addition, the ultraviolet and fluorescence response of the HL1 and HL2 shown marked changes upon their complexation with Cr(III) ion, which indicated that the two 8-hydroxyquinolinate based ligand are promising heavy metal chelating agent for Cr3+. Full article
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Open AccessArticle New Developments in Cathodoluminescence Spectroscopy for the Study of Luminescent Materials
Materials 2017, 10(3), 312; https://doi.org/10.3390/ma10030312
Received: 22 January 2017 / Revised: 7 March 2017 / Accepted: 15 March 2017 / Published: 17 March 2017
Cited by 2 | PDF Full-text (4578 KB) | HTML Full-text | XML Full-text
Abstract
Herein, we describe three advanced techniques for cathodoluminescence (CL) spectroscopy that have recently been developed in our laboratories. The first is a new method to accurately determine the CL-efficiency of thin layers of phosphor powders. When a wide band phosphor with a band
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Herein, we describe three advanced techniques for cathodoluminescence (CL) spectroscopy that have recently been developed in our laboratories. The first is a new method to accurately determine the CL-efficiency of thin layers of phosphor powders. When a wide band phosphor with a band gap (Eg > 5 eV) is bombarded with electrons, charging of the phosphor particles will occur, which eventually leads to erroneous results in the determination of the luminous efficacy. To overcome this problem of charging, a comparison method has been developed, which enables accurate measurement of the current density of the electron beam. The study of CL from phosphor specimens in a scanning electron microscope (SEM) is the second subject to be treated. A detailed description of a measuring method to determine the overall decay time of single phosphor crystals in a SEM without beam blanking is presented. The third technique is based on the unique combination of microscopy and spectrometry in the transmission electron microscope (TEM) of Brunel University London (UK). This combination enables the recording of CL-spectra of nanometre-sized specimens and determining spatial variations in CL emission across individual particles by superimposing the scanning TEM and CL-images. Full article
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