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High temperature creep of 20 vol%. SiC-HfB2 UHTCs up to 2000 degrees C and the effect of La2O3 addition

Zapata-Solvas, E; Gomez-Garcia, D; Dominguez-Rodriguez, A; Lee, WE
Journal of the European Ceramic Society. 38 (2018) 47-56


High temperature compressive creep of SiC-HfB2 UHTCs up to 2000 °C has been studied. Microstructural analysis after deformation reveals formation of new phases in the Hf-B-Si and Hf-B-Si-C systems, which are responsible for the poor creep resistance. RE oxide additions have a negative effect reducing the creep resistance of SiC-HfB2 UHTCs. A simplistic analysis for the required creep resistance is described, indicating that only SiC-HfB2 UHTCs could withstand re-entry conditions for 5 min in a single use. However, RE oxide addition to SiC-HfB2UHTCs does not provide the required creep resistance for them to be candidate materials for hypersonic applications.

Enero, 2018 | DOI: 10.1016/j.jeurceramsoc.2017.08.028

Packing Defects in Fatty Amine Self-Assembled Monolayers on Mica as Revealed from AFM Techniques

Benitez, JJ; Heredia-Guerrero, JA; San-Miguel, MA; Galloway, HC
Journal of Physical Chemistry B, 122 (2018) 493-499


Self-assembled monolayers of n-octadecylamine (ODA-SAMs) on mica have been prepared and studied by contact and jumping mode atomic force microscopy (AFM). Adhesion and friction data show that the compactness of the monolayers spontaneously increases as they are allowed to ripen. Molecular packing can also be induced by the controlled mechanical perturbation exerted by the probe when getting into and out of contact intermittently. Under these conditions, defects and vacancies aggregate giving rise to detectable pinholes uniformly distributed in AFM images. Created pinhole density was found to decrease with ripening time, thus confirming the proposed spontaneous self-healing mechanism. Pinhole density is also suggested as a parameter characterizing the packing degree of ODA-SAMs, and it has been related to their tribological properties. Additionally, molecular dynamics simulations were used to corroborate the compatibility between the packing degree and the observed topography of ODA-SAMs on mica.

Enero, 2018 | DOI: 10.1021/acs.jpcb.7b03603

Nickel Particles Selectively Confined in the Mesoporous Channels of SBA-15 Yielding a Very Stable Catalyst for DRM Reaction

Rodriguez-Gomez, A; Pereniguez, R; Caballero, A
Journal of Physical Chemistry B, 122 (2018) 500-510


A series of four Ni catalysts supported on SBA-15 and on a high SiO2 surface area have been prepared by modified impregnation (ImU) and deposition-precipitation (DP) methods. The catalysts have been extensively characterized, including in situ XAS (bulk sensitive) and XPS (surface sensitive) techniques, and their catalytic activities evaluated in the dry reforming reaction of methane (DRM). The combined use of XPS and XAS has allowed us to determine the location of nickel particles on each catalyst after reduction at high temperature (750 degrees C). Both Ni/SiO2-DP and Ni/SBA-15-DP catalysts yield well-dispersed and homogeneous metallic phases mainly located in the mesoporosity of both supports. On the contrary, the Ni/SiO2-ImU and Ni/SBA-15-ImU catalysts present a bimodal distribution of the reduced nickel phase, with nickel metallic particles located out and into the mesoporous structure of SiO2 or the SBA-15 channels. The Ni/SBA-15-DP catalyst was found the most stable and performing system, with a very low level of carbon deposition, about an order of magnitude lower than the equivalent ImU catalyst. This outstanding performance comes from the confinement of small and homogeneous nickel particles in the mesoporous channels of SBA-15, which, in strong interaction with the support, are resistant to sintering and coke deposition during the demanding reaction conditions of DRM.

Enero, 2018 | DOI: 10.1021/acs.jpcb.7b03835

A new combustion route for synthesis of TaB2 nanoparticles

Jalaly, M; Gotor, FJ
Ceramics International, 44 (2018) 1142-1146


Tantalum diboride (TaB2) nanoparticles were synthesized through a mechanically induced self-sustaining reaction (MSR). In this method, the ternary system of Mg/Ta2O5/B was employed in which, magnesium was used as a reducing agent for reduction of tantalum oxides in a combustive regime. The processing route of TaB2 by the solid-state combustion was very short-term and the product purification was extremely easy and rapid. The synthesis mechanism was studied and revealed that magnesiothermic reduction of tantalum oxide is the initiator of the total reaction, while borothermic reduction of the oxide may occur in parallel.

Enero, 2018 | DOI: 10.1016/j.ceramint.2017.10.074

Nickel/Copper Bilayer-modified Screen Printed Electrode for Glucose Determination in Flow Injection Analysis

Salazar, P.; Rico, V.; Gonzalez-Elipe, Agustin R.
Electroanalysis, 30 (2018) 187-193


This work reports about the performance of a Ni/Cu-modified screen printed electrodes (SPE/Ni/Cu), prepared by physical vapor deposition (PVD) in an oblique angle configuration (OAD), for non-enzymatic glucose sensing applications. SPE/Ni/Cu electrodes showed an excellent reversibility and a catalytic behavior for detection of glucose that were controlled by the diffusion of reactants up to the active sites at the electrode surface. The study with a flow injection analysis (FIA) setup of the main experimental variables affecting the detection process has shown that the developed electrode system had an excellent glucose sensitivity of 1.04AM(-1)cm(-2) (R-2:0.999), a linear response up to 1mM, a limit of detection of 0.33M and a time of analysis of ca. 30s per sample. The selectivity of the sensor was checked against various interferences, including ascorbic acid, uric acid, acetaminophen and other sugars, in all cases with excellent results. The feasibility of using this sensor for practical applications was successfully confirmed by determining the glucose concentration in different commercial beverages.

Enero, 2018 | DOI: 10.1002/elan.201700592

Development of a novel fcc structure for an amorphous-nanocrystalline Ti-33Nb-4Mn (at.%) ternary alloy

Chicardi, E; Garcia-Garrido, C; Sayagues, MJ; Torres, Y; Amigo, V; Aguilar, C
Materials Characterization, 135 (2018) 46-56


In this work, a novel amorphous-nanocrystalline titanium-niobium-manganese solid solution ternary alloy with a Ti-33Nb-4Mn (at.%) nominal composition was developed by a High-Energy Mechanical Alloying. Nb and Mn were added to the elemental Ti as a beta-phase (bcc) stabilizer and an amorphization promoter, respectively. The system evolved from the elemental Ti, Nb and Mn raw materials to a body centred cubic (bcc) TiNbMn alloy and, finally, to the formation of an original and stable face centred cubic (fcc) nanocrystalline TiNbMn alloy, not reported until now, at short milling time (20 h). This alloy remains invariant until 120 h. In turn, the partial amorphization of the system occurs and increases until at intermediate milling time (80 h). The production of both original fcc and the amorphous TiNbMn alloy may be beneficial for reducing the Young's modulus and improving the mechanical strength pursued for the Ti alloy. The optimal milling time respect to the amorphization, nanocrystalline size and Fe mount from milling media was 60 h and 80 h (TiNbMn60h and TiNbMn80h), with > 50 wt% of an amorphous phase and a crystalline domain size of approximately 5 nm.

Enero, 2018 | DOI: 10.1016/j.matchar.2017.11.021

A facile shape-controlled synthesis of highly photoactive fluorine containing TiO2 nanosheets with high {001} facet exposure

Lara, M. A.; Sayagues, M. J.; Navio, J. A.; Hidalgo, M. C.
Journal of Materials Science, 53 (2018) 435-446


Surface-fluorinated TiO2 materials with high {001} facet exposure were prepared by a simple and high-yield preparation procedure. Faceted/fluorinated samples showed a high photocatalytic performance not only in oxidation processes, tested in phenol and methyl orange degradation, but also in a reduction process as Cr(VI) photoreduction. Reaction rates for these materials greatly exceeded the ones obtained for materials prepared without fluorine addition and for commercial TiO2 Degussa (Evonik) P25 used as reference photocatalyst. A broad characterisation of the samples allowed us to estimate the percentages of different facets and the amount and form in which the fluorine is found on the surfaces. Good photocatalytic behaviour can be ascribed to both high {001} facet exposure and adsorbed fluorine on the photocatalysts surfaces.

Enero, 2018 | DOI: 10.1007/s10853-017-1515-6

Core-rim structure formation in TiC-Ni based cermets fabricated by a combined thermal explosion/hot-pressing process

Lemboub, S; Boudebane, S; Gotor, FJ; Haouli, S; Mezrag, S; Bouhedja, S; Hesser, G; Chadli, H; Chouchane, T
International Journal of Refractory Metals & Hard Materials, 70 (2018) 84-92


TiC-Ni-based cermets were obtained by thermal explosion from different elemental mixtures (Ti, C, Ni and X, where X = Cr, Mo or W) and subsequently densified by hot-pressing under a cyclic load. The whole process was performed in a single stage in the same experimental device according to the following thermal and pressure procedure: a heating rate ramp up to 1573 K without applying any load followed by an isothermal dwelling under a compressive cyclic load of 32 MPa. The thermal explosion synthesis occurred during the heating ramp at a temperature close to 1273 K that was practically independent of the starting nominal composition. The influence of different refractory elements on the chemical composition and microstructure of cermets was studied. SEM characterization showed that only with Mo and W, the cermets developed the characteristic core-rim structure. A high densification was achieved, but decreased when the refractory elements were added. Nevertheless, in these cases higher hardness values were obtained.

Enero, 2018 | DOI: 10.1016/j.ijrmhm.2017.09.014

The dizinc bond as a ligand: A computational study of elongated dizinc bonds

Ayala, R; Carmona, E; Galindo, A
Inorganic Chimica Acta, 470 (2018) 197-205


Following the synthesis of [Zn-2(eta(2)-C5Me5)(2)] (in short [Zn2Cp*(2)]) many complexes of the directly bonded Zn-Zn unit were prepared and characterized, leading to the recognition of an isolobal analogy between the Zn-Zn bond and the molecule of dihydrogen. Prompted by these results, we have investigated eta(2)-eta(2)-coordination of [Zn2Cp2] and [Zn2Ph2] (Cp = C5H5, Ph = C6H5) to several selected transition metal fragments and report herein the results of a QTAIM study of complexes [(ZnR)(2)Fe(CO)(4)], [(eta(2)-Zn2R2)M(CO)(5)]] and [(eta(2)-Zn2R2)Pd(PR'(3))(2)] (for R = Cp, Ph; M = Cr, Mo, W; and R' = F, H, Me). A decrease of rho(BCP), Delta(2) rho(BCP) and delocalization indexes delta(Zn, Zn), relative to corresponding values in the parent molecules of [Zn2Cp2] and [Zn2Ph2], accompanied dizinc coordination. In most cases the computed d(Zn, Zn) parameters were indicative of significant electron density sharing between the two Zn atoms. Nevertheless, the interaction with [Fe(CO)(4)] resulted in oxidative cleavage of the coordinated Zn-Zn bond, due to high pi backdonation to the sigma* Zn-2 MO as deduced from the delta(M, O-CO) index. The Zn-Zn bond critical points identified in our study are discussed. The computed Zn-Zn contacts concentrate in the range 2.44-2.58 angstrom, and we propose that this interval corresponds to elongated dizinc bonds. 

Enero, 2018 | DOI: 10.1016/j.ica.2017.06.008


Fluorescent Humidity Sensors Based on Photonic Resonators

Szendrei, K; Jimenez-Solano, A; Lozano, G; Lotsch, BV; Miguez, H
Advanced Optical Materials, 5 (2017) 1700663


Among the different approaches to humidity sensing available, those based on fluorescent signals are gathering a great deal of attention due to their fast response and versatility of detection and design. So far, all proposals have focused on the use of luminescent probes whose emission is either triggered or inhibited by the presence of water that reacts or alters their chemical environment, hence inducing the signal change. Here, a novel concept in fluorescent humidity sensing based on combining stimuli-responsive photonic resonators with molecular fluorescent probes is introduced. The resonator is assembled from humidity-swellable antimony phosphate nanosheets embedding a planar light-emitting probe, whose emission is dramatically modified by the changes that ambient humidity causes in its photonic environment. Guided by "in silico" optical design of the resonator architecture and subsequent experimental realization, two embodiments of fluorescent photonic humidity sensors featuring turn-on and turn-off detection schemes are presented. The interplay between the luminescent properties of an emitter and its photonic environment implies a fundamental advantage as the emitters are not chemically altered during the detection process. At the same time, it paves the way toward a new generation of photonic humidity sensors which can conveniently be interfaced with common fluorescence detection schemes.

Diciembre, 2017 | DOI: 10.1002/adom.201700663

Local Disorder and Tunable Luminescence in Sr1–x/2Al2–xSixO4 (0.2 ≤ x ≤ 0.5) Transparent Ceramics

Fernandez-Carrion, AJ; Al Saghir, K; Veron, E; Becerro, AI; Porcher, F; Wisniewsld, W; Matzen, G; Fayon, F; Allix, M
Inorganic Chemistry, 56 (2017) 14446-14458


Eu-doped Sr1–x/2Al2–xSixO4 (x = 0.2, 0.4, and 0.5) transparent ceramics have been synthesized by full and congruent crystallization from glasses prepared by aerodynamic levitation and laser-heating method. Structural refinements from synchrotron and neutron powder diffraction data show that the ceramics adopt a 1 × 1 × 2 superstructure compared to the SrAl2O4 hexagonal polymorph. While the observed superstructure reflections indicate a long-range ordering of the Sr vacancies in the structure, 29Si and 27Al solid-state NMR measurements associated with DFT computations reveal a significant degree of disorder in the fully polymerized tetrahedral network. This is evidenced through the presence of Si–O–Si bonds, as well as Si(OAl)4 units at remote distances of the Sr vacancies and Al(OAl)4 units in the close vicinity of Sr vacancies departing from local charge compensation in the network. The transparent ceramics can be doped by europium to induce light emission arising from the volume under UV excitation. Luminescence measurements then reveal the coexistence of Eu2+ and Eu3+ in the samples, thereby allowing tuning the emission color depending on the excitation wavelength and suggesting possible applications such as solid state lighting.

Diciembre, 2017 | DOI: 10.1021/acs.inorgchem.7b01881

Calcium-Looping performance of steel and blast furnace slags for thermochemical energy storage in concentrated solar power plants

Valverde, JM; Miranda-Pizarro, J; Perejon, A; Sanchez-Jimenez, PE; Perez-Maqueda, LA
Journal of CO2 Utilization, 22 (2017) 143-154


The Calcium Looping (CaL) process, based on the carbonation/calcination of CaO, has been proposed as a feasible technology for Thermochemical Energy Storage (TCES) in Concentrated Solar Power (CSP) plants. The CaL process usually employs limestone as CaO precursor for its very low cost, non-toxicity, abundance and wide geographical distribution. However, the multicycle activity of limestone derived CaO under relevant CaL conditions for TCES in CSP plants can be severely limited by pore plugging. In this work, the alternative use of calcium-rich steel and blast furnace slags after treatment with acetic acid is investigated. A main observation is that the calcination temperature to regenerate the CaO is significantly reduced as compared to limestone. Furthermore, the multicycle activity of some of the slags tested at relevant CaL conditions for TCES remains high and stable if the treated samples are subjected to filtration. This process serves to remove silica grains, which helps decrease the porosity of the CaO resulting from calcination in the mesoporous range thus mitigating pore plugging.

Diciembre, 2017 | DOI: 10.1016/j.jcou.2017.09.021

Performance of biomorphic Silicon Carbide as particulate filter in diesel boilers

Orihuela, M Pilar; Gomez-Martin, Aurora; Becerra, Jose A; Chacartegui, Ricardo; Ramirez-Rico, Joaquin
Journal of Environmental Management, 203 (2017) 907-919


Biomorphic Silicon Carbide (bioSiC) is a novel porous ceramic material with excellent mechanical and thermal properties. Previous studies have demonstrated that it may be a good candidate for its use as particle filter media of exhaust gases at medium or high temperature. In order to determine the filtration efficiency of biomorphic Silicon Carbide, and its adequacy as substrate for diesel particulate filters, different bioSiC-samples have been tested in the flue gases of a diesel boiler. For this purpose, an experimental facility to extract a fraction of the boiler exhaust flow and filter it under controlled conditions has been designed and built. Several filter samples with different microstructures, obtained from different precursors, have been tested in this bench. The experimental campaign was focused on the measurement of the number and size of particles before and after placing the samples. Results show that the initial efficiency of filters made from natural precursors is severely determined by the cutting direction and associated microstructure. In biomorphic Silicon Carbide derived from radially cut wood, the initial efficiency of the filter is higher than 95%. Nevertheless, when the cut of the wood is axial, the efficiency depends on the pore size and the permeability, reaching in some cases values in the range 70–90%. In this case, the presence of macropores in some of the samples reduces their efficiency as particle traps. In continuous operation, the accumulation of particles within the porous media leads to the formation of a soot cake, which improves the efficiency except in the case when extra-large pores exist. For all the samples, after a few operation cycles, capture efficiency was higher than 95%. These experimental results show the potential for developing filters for diesel boilers based on biomorphic Silicon Carbide.

Diciembre, 2017 | DOI: 10.1016/j.jenvman.2017.05.003

High temperature compressive strength and creep behavior of Si-Ti-C-O fiber-bonded ceramics

Vera, MC; Martinez-Fernandez, J; Singh, M; Ramirez-Rico, J
Journal of the European Ceramic Society, 37 (2017) 4442-4448


Fiber bonded silicon carbide ceramic materials provide cost-advantage over traditional ceramic matrix composites and require fewer processing steps. Despite their interest in extreme environment thermostructural applications no data on long term mechanical reliability other than static fatigue is available for them. We studied the high temperature compressive strength and creep behavior of a fiber bonded SiC material obtained by hot-pressing of Si Ti-C-O fibers. The deformation mechanism and onset of plasticity was evaluated and compared with other commercial SiC materials. Up to 1400 degrees C, plasticity is very limited and any macroscopic deformation proceeds by crack formation and damage propagation. A transient viscous creep stage is observed due to flow in the silica matrix and once steady state is established, a stress exponent n similar to 4 and an activation energy Q similar to 700 kJ mol(-1) are found. These results are consistent with previous data on creep of polymer derived SiC fibers and polycrystals.

Diciembre, 2017 | DOI: 10.1016/j.jeurceramsoc.2017.06.037

Silver and gold nanoparticles in nanometric confined templates: synthesis and alloying within the anisotropic pores of oblique angle deposited films

Parra-Barranco, J., Sánchez-Valencia, J.R., Barranco, A., González-Elipe, A.R.
Nanotechnology, 28 (2017) 485602


In this work we have developed an infiltration methodology to incorporate metal nanoparticles (NPs) of controlled size and shape into the open voids available in oblique angle deposited thin films. These NPs exhibited well-defined surface plasmon resonances (SPRs). The nanometric confined space provided by their porous microstructure has been used as a template for the growth of anisotropic NPs with interesting SPR properties. The fabrication methodology has been applied for the preparation of films with embedded Ag and Au NPs with two associated plasmon resonance features that developed a dichroic behaviour when examined with linearly polarized light. A confined alloying process was induced by near IR nanosecond laser irradiation yielding bimetallic NPs with SPR features covering a large zone of the electromagnetic spectrum. The possibilities of the method for the tailored fabrication of a wide range colour palette based on SPR features are highlighted.

Diciembre, 2017 | DOI: 10.1088/1361-6528/aa92af

Effect of acid-treatment and colloidal-processing conditions on the room temperature mechanical and electrical properties of 3YTZP/MWNT ceramic nanocomposites

Poyato, R.; Morales-Rodríguez, A.; Gutiérrez-Mora, F.; Muñoz, A.; Gallardo-López, A.
Ceramics International, 43 (2017) 16560-16568


Different colloidal powder processing routines have been used to prepare composites of 3 mol% Y2O3 -ZrO2 (tetragonal zirconia polycrystals, 3YTZP) with 2.5 vol% multiwall carbon nanotubes (MWNT) with the aim of achieving a homogeneous distribution of the MWNTs in the ceramic, eliminating agglomerates but also minimizing carbon nanotube (CNT) damage during processing. Modifications of the acid treatment applied to the nanotubes, including subjecting them to stirring or ultrasonic agitation, and use of acid or basic pH during composite powder mixing have been approached.
No MWNT damage during processing was detected by Raman spectroscopy. CNT bundles were found in all the composites forming different patterns depending on the processing route. Similar values of hardness were obtained for all the composites, while different anisotropy in fracture propagation was found when studying parallel and perpendicular directions to the sintering pressing axis on the cross sections of the composites due to the MWNT preferential alignment. The CNT bundles were found to act as fracture short paths. A similar anisotropic behavior was observed for the electrical conductivity. These results have been correlated to the different microstructures obtained in the composites prepared with different processing routines.

Diciembre, 2017 | DOI: 10.1016/j.ceramint.2017.09.043

Micron-scale wedge thin films prepared by plasma enhanced chemical vapor deposition

Lopez-Santos, MC; Alvarez, R; Palmero, A; Borras, A; del Campo, RC; Holgado, M; Gonzalez-Elipe, AR
Plasma Processes and Polymers, 14 (2017) e1700043


Wedge-shaped materials are currently employed for optical analyses and sensing applications. In this paper, we present an easy to implement plasma enhanced chemical vapor deposition procedure to grow wedge-shaped thin films with controlled slope at the scale of few hundred microns. The method relies on the use of few tenths micron height obstacles to alter the laminar flow of precursor gas during deposition and is applied for the fabrication of wedge-shaped ZnO thin films. Local interference patterns, refractive index, and birefringence of the films have been measured with one micron resolution using a specially designed optical set-up. Their micro- and nano-structures have been characterized by means of scanning electron microscopy and theoretically reproduced by Monte Carlo calculations.

Diciembre, 2017 | DOI: 10.1002/ppap.201700043

Photochemical methane partial oxidation to methanol assisted by H2O2

López Martin, A.; Caballero, A.; Colón, G.
Journal of Photochemistry and Photobiology A: Chemistry, 349 (2017) 216-223


The photochemical conversion of methane into methanol from H2O2 aqueous solution as well as the effect of the addition mode were studied. Direct addition of different amounts H2O2 leads to increasing methanol production at the first stage of the reaction. The excess of H2O2 would lead to the reactive oxygen species scavenging and the subsequent O2 production. It was also corroborated that extra hydroxyl radicals in the aqueous medium do not improve the formation of methanol but a noticeable increase in the formation of HCOOH with respect to methanol was evidenced. In contrast, dosing addition at relatively low rates leads to constant methane consumption towards methanol. Methanol formation would be in this case in equilibrium with further oxidation to HCOOH or CO2. This suggests that only a controlled constant availability of HO’s at low concentration can enhance the performance of methanol generation in the photochemical process.

Diciembre, 2017 | DOI: 10.1016/j.jphotochem.2017.09.039

Microemulsion-Mediated Synthesis and Properties of Uniform Ln:CaWO4 (Ln = Eu, Dy) Nanophosphors with Multicolor Luminescence for Optical and CT Imaging

Laguna, M; Nuñez, NO; Garcia, FJ; Corral, A; Parrado-Gallego, A; Balcerzyk, M; Becerro, AI; Ocaña, M
European Journal of Inorganic Chemistry, 44 (2017) 5158-5168


A new room-temperature method has been developed that yields, for the first time in the literature, uniform and well-dispersed CaWO4 nanospindles. This method is based on the use of microemulsions consisting of aqueous solutions of Ca2+ and WO42- precursors, cyclohexane as the organic medium, Triton X-100 as the surfactant, and n-octanol as the cosurfactant. We show that the formation of uniform nanospindles requires a restrictive set of experimental conditions. These particles crystallize into the tetragonal CaWO4 phase and emit blue-green luminescence when excited by UV radiation. The reported method is also useful for doping the CaWO4 spindles with Eu3+ or Dy3+ cations, resulting in multicolor emissions (red for Eu3+; white for Dy3+). The luminescence is much stronger when excited through a WO42--Ln(3+) (Ln = Eu or Dy) energy-transfer band than through the f-f transition bands of the Ln(3+) cations. Interestingly, because of the white luminescence associated with the Dy:CaWO4 nanophosphor, it might be useful for LED technologies. Luminescence dynamics and energy-transfer efficiency have been analyzed to determine the optimum phosphors. Finally, the Eu-doped CaWO4 nanospindles also showed excellent X-ray attenuation efficacy, which confers double functionality to this material as both a luminescence bioprobe and as a contrasting agent for X-ray computed-tomography.

Diciembre, 2017 | DOI: 10.1002/ejic.201700650

Chalcogenide Quaternary Cu2FeSnS4 Nanocrystals for Solar Cells: Explosive Character of Mechanochemical Synthesis and Environmental Challenge

Balaz, P; Balaz, M; Sayagues, MJ; Eliyas, A; Kostova, NG; Kanuchova, M; Dutkova, E; Zorkovska, A
Crystals, 7 (2017) art. 367


In this study we demonstrate the synthesis of quaternary semiconductor nanocrystals of stannite Cu2FeSnS4/rhodostannite Cu2FeSn3S8 (CFTS) via mechanochemical route using Cu, Fe, Sn and S elements as precursors in one-pot experiments. Methods of X-ray diffraction (XRD), nitrogen adsorption, high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) were applied to characterize properties of the unique nanostructures. Mechanochemical route of synthesis induced new phenomena like explosive character of reaction, where three stages could be identified and the formation of nanostructures 5-10 nm in size. By using XPS method, Cu(I), Fe(II), Sn(IV) and S(-II) species were identified on the surface of CFTS. The value of optical band gap 1.27 eV is optimal for semiconductors applicable as absorbers in solar cells. The significant photocatalytic activity of the CFTS nanocrystals was also evidenced. The obtained results confirm the excellent properties of the quaternary semiconductor nanocrystals synthesized from earth-abundant elements.

Diciembre, 2017 | DOI: 10.3390/cryst7120367