National Institute Of Materials Physics - Romania

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31. Bulk and surface characteristics of co-electrodeposited Cu2FeSnS4 thin films sulfurized at different annealing temperatures
Authors: El Khouja, O; Negrila, CC; Nouneh, K; Secu, M; Touhami, ME; Matei, E; Stancu, V; Enculescu, M; Kuncser, V; Galca, AC

Published: JUN 15 2022, JOURNAL OF ALLOYS AND COMPOUNDS, 906, 164379, DOI: 10.1016/j.jallcom.2022.164379

In this study, stannite, Cu2FeSnS4 (CFTS), absorber films were obtained by electrodeposition on Molybdenum-coated soda-lime substrates, followed by sulfurization treatment at certain temperatures in the 400-550 degrees C range. The purposes of this work were to control the manufacturing of CFTS films with good stoichiometry, high crystallinity and to study the annealing temperature impact on CFTS films properties. The X-ray diffraction and the Raman spectroscopy measurement distinguished the CFTS phase formation, with a presence of SnS2 secondary phase. The energy dispersive spectroscopy results reveal compositional differences between samples as well as the in-depth gradients. The photoluminescence emission band around 1.35-1.40 eV is slightly below the direct bandgap inferred from the conventional spectroscopy (diffuse reflectance). X-ray photoelectron spectroscopy results indicate clearly a high amount of Sn on the surface. The Conversion Electron Mossbauer unveiled the presence of Fe in the chalcogenide unit cell. The electrochemical characteristics of the synthesized films are also given. (c) 2022 Elsevier B.V. All rights reserved.
32. Enhanced magnetocaloric properties of La0.8K0.2-xPbxMnO3 nanoparticles by optimizing Pb doping concentrations
Authors: Bouzid, SA; Essoumhi, A; Rostas, AM; Kuncser, AC; Negrila, CC; Iacob, N; Galatanu, A; Popescu, B; Sajieddine, M; Galca, AC; Kuncser, V

Published: JUN 15 2022, CERAMICS INTERNATIONAL, 48, DOI: 10.1016/j.ceramint.2022.02.239

Polycrystalline La(0.8)K(0.2-x)Pb(x)MnO3 (x = 0.05, 0.10, 0.15, 0.20) ceramics were successfully prepared by flash combustion route and their structural, morphological, magnetic and magnetocaloric properties were investi-gated. Structural analyses using X-ray diffraction reveal that all samples are crystallized in the rhombohedral structure and belong to R <(3) over bar > c space group. The increase of Pb doping does not modify the crystalline structure but changes the grain size and lattice parameters. X-ray photoelectron spectroscopy (XPS) fitting results of Mn 2p peaks confirmed the coexistence of Mn3+ and Mn4+ ions which contribute to the double exchange interactions improving the ferromagnetic order in the samples. The magnetization's temperature and magnetic field de-pendences indicate a second-order ferromagnetic-paramagnetic transition of the ceramics. A significant mag-netic entropy change near room temperature was observed for La0.8K0.1Pb0.1MnO3, showing considerable magnetocaloric properties. Furthermore, electron paramagnetic resonance spectroscopy (EPR) was also used to examine the ferromagnetic-paramagnetic transition.
33. Effect of chlorine and bromine on the perovskite crystal growth in mesoscopic heterojunction photovoltaic device
Authors: Mehdi, H; Leonat, LN; Stancu, V; Saidi, H; Enculescu, M; Tomulescu, AG; Toma, V; Pintilie, I; Bouazizi, A; Galca, AC

Published: JUN 1 2022, MATERIALS SCIENCE IN SEMICONDUCTOR PROCESSING, 143, 106558, DOI: 10.1016/j.mssp.2022.106558

Organic-inorganic hybrid perovskite solar cells are within the emerging photovoltaic technologies. The combination of different halogen ions, in certain fill fractions, is one of the methods to improve the perovskite film properties. Herein, fabrication and characterization of perovskite cells in standard mesoscopic architecture using one-step deposition method has been done. The role of the halogen ions (Chlorine or Bromine) on crystal structure growth and photoelectric performance has been investigated. X-ray diffraction, scanning electron microscopy, atomic force microscopy and optical microscopy analysis were performed. The microstructure, composition and morphology of CH3NH3PbI1.8Br1.2 and CH3NH3PbI1.8Cl1.2 films are dissimilar, although identical fabrication method was used. Same holds for optical properties, band gap energies of 1.84 eV and 1.63 eV, respectively, being obtained. Integrated in solar cells, the maximum power conversion efficiency of the Br based devices is beyond 10%, while for those based on Cl, the efficiency drops around 5%.
34. A Two-Step Magnetron Sputtering Approach for the Synthesis of Cu2ZnSnS4 Films from Cu2SnS3\ZnS Stacks
Authors: Zaki, MY; Sava, F; Simandan, ID; Buruiana, AT; Stavarache, I; Bocirnea, AE; Mihai, C; Velea, A; Galca, AC

Published: JUN 2022, ACS OMEGA, DOI: 10.1021/acsomega.2c02475

Cu2ZnSnS4 (CZTS) is regarded as one of the emerging materials for next-generation thin film solar cells. However, its synthesis is complex, and obtaining a single-phase CZTS thin film is difficult. This work reports the elaboration of Cu2ZnSnS4 thin films by a sequential magnetron sputtering deposition of Cu2SnS3 (CTS) and ZnS as stacked films. Initially, the CTS films were prepared on a soda lime glass substrate by annealing Cu and SnS2 stacked layers. Second, ZnS was deposited by magnetron sputtering on the CTS films. The CTS\ZnS stacks were then annealed in Sn + S or S atmospheres. The tetragonal CZTS structure was obtained and confirmed by grazing incidence X-ray diffraction and Raman spectroscopy. The morphological and compositional characteristics, measured by scanning electron microscopy and energy-dispersive spectroscopy, revealed large grains and dense surfaces with the elemental composition close to the intended stoichiometry. Additional X-ray photoemission spectroscopy measurements were performed to determine the surface chemistry and particularities of the obtained films. The optical properties, determined using conventional spectroscopy, showed optimal absorber layer band gap values ranging between 1.38 and 1.50 eV. The electrical measurements showed that all the films are p-type with high carrier concentrations in the range of 10(15) to 10(20) cm(-3). This new synthesis route for CZTS opens the way to obtain high-quality films by an industry-compatible method.
35. Effect of the stacking order, annealing temperature and atmosphere on crystal phase and optical properties of Cu2SnS3
Authors: Zaki, MY; Sava, F; Simandan, ID; Buruiana, AT; Mihai, C; Velea, A; Galca, AC

Published: MAY 13 2022, SCIENTIFIC REPORTS, 12, 7958, DOI: 10.1038/s41598-022-12045-3

Cu2SnS3 (CTS) is emerging as a promising absorber for the next generation thin film solar cells (TFSC) due to its excellent optical and electronic properties, earth-abundance and eco-friendly elemental composition. In addition, CTS can be used as precursor films for the Cu2ZnSnS4 (CZTS) synthesis. The optical properties of CTS are influenced by stoichiometry, crystalline structure, secondary phases and crystallite size. Routes for obtaining CTS films with optimized properties for TFSC are still being sought. Here, the CTS thin films synthesized by magnetron sputtering on soda lime glass (SLG) using Cu and SnS2 targets in two different stacks, were studied. The SLG\Cu\SnS2 and SLG\SnS2\Cu stacks were annealed in S and Sn + S atmospheres, at various temperatures. Both stacks show a polymorphic structure, and higher annealing temperatures favor the monoclinic CTS phase formation. Morphology is influenced by the stacking order since a SnS2 top layer generates several voids on the surface due to the evaporation of SnS, while a Cu top layer provides uniform and void-free surfaces. The films in the copper-capped stack annealed under Sn + S atmosphere have the best structural, morphological, compositional and optical properties, with tunable band gaps between 1.18 and 1.37 eV. Remarkably, secondary phases are present only in a very low percent (< 3.5%) in samples annealed at higher temperatures. This new synthesis strategy opens the way for obtaining CTS thin films for solar cell applications, that can be used also as intermediary stage for CZTS synthesis.
36. ZnS stacking order influence on the formation of Zn-poor and Zn-rich Cu2ZnSnS4 phase
Authors: Zaki, MY; El Khouja, O; Nouneh, K; Touhami, ME; Matei, E; Azmi, S; Rusu, MI; Grigorescu, CEA; Briche, S; Boutamart, M; Badica, P; Burdusel, M; Secu, M; Pintilie, L; Galca, AC

Published: MAY 2022, JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS, 33, DOI: 10.1007/s10854-022-08160-6

This paper reports the synthesis and characterization of Cu2ZnSnS4 (CZTS) absorber films, prepared by a two-step electrodeposition of a ZnS (zinc sulfide) binary and a CZT (copper, zinc and tin) ternary precursors on Mo/Ti/Si substrates. The as-electrodeposited ZnS/CZT and CZT/ZnS stacks were thermally treated in a tubular furnace in sulfur environment at 550 degrees C. The role of the ZnS buffer layer is to provide a zinc and sulfur reservoir, needed to complete the formation of kesterite phase. X-ray diffraction and Raman analyses revealed the formation of the CZTS phase. The surface morphology and chemical composition of the films were studied using a scanning electron microscope. The bandgap values inferred from diffuse reflectance data, are discussed with respect to the stoichiometry which is considerably affected by the order of the stacks. Room-temperature photoluminescence of the CZT/ZnS sample showed a board PL band of 1.51 eV. It was found that the film with a ZnS layer on top is preferred for the formation of a Zn-rich single CZTS phase.
37. Nanoscopic correlations from curve fitting of photoelectron spectromicroscopy data cubes of lead zirconate titanate films
Authors: Abramiuc, LE; Tanase, LC; Barinov, A; Chirila, CF; Teodorescu, CM

Published: MAY 2022, RESULTS IN PHYSICS, 36, 105436, DOI: 10.1016/j.rinp.2022.105436

Photoelectron spectromicroscopy data cubes with sub-micrometer spatial resolution from a lead zirconate titanate thin film are fitted in each spatial point for several areas investigated, and correlations between the results of the fitting parameters are established, enabling one to suggest that surface band bending manifests also in the case of samples with multiple polarization states. These surface band bendings may be used for preliminary assessment of polarization states by using the contrast in binding energy. However, the individual curve fitting of each spectrum and the analysis of correlations between the derived parameters (binding energies and amplitudes) yields results of deeper significance in deriving the distribution of band bending. This allows in some cases discriminating between the origin of the individual components, assessing charging effects and compensation mechanisms, also enabling one to establish correlations between areas with different polarization. It is found that the major part of the investigated areas consist in regions with outwards polarization and without out-of-plane polarization, with the presence of some isolated metal Pb clusters. On a single area, components attributed to inwards polarization are detected, and their formation occurs at the expense of areas without out-of-plane polarization, mostly for a given proportion of the outwards polarization.
38. Electrode dependence of polydomain stability in ferroelectric thin films
Authors: Misirlioglu, IB; Pintilie, L

Published: MAY 2022, SCRIPTA MATERIALIA, 213, 114589, DOI: 10.1016/j.scriptamat.2022.114589

39. Electrochemical and In Vitro Biological Evaluation of Bio-Active Coatings Deposited by Magnetron Sputtering onto Biocompatible Mg-0 .8Ca Alloy
Authors: Bita, AI; Antoniac, I; Miculescu, M; Stan, GE; Leonat, L; Antoniac, A; Constantin, B; Forna, N

Published: MAY 2022, MATERIALS, 15, 3100, DOI: 10.3390/ma15093100

The use of resorbable magnesium alloys in the design of implants represents a new direction in the healthcare domain. Two main research avenues are currently explored for developing or improving metallic biomaterials: (i) increase of their corrosion resistance by designed compositional and structural modifications, and (ii) functionalization of their surfaces by coating with ceramic or polymeric layers. The main objective of this work was to comparatively assess bio-functional coatings (i.e., highly-crystallized hydroxyapatite and silica-rich glass) deposited by radio-frequency magnetron sputtering (RF-MS) on a biodegradable Mg-0.8Ca alloy (0.8 wt.% of Ca). After probing their morphology (by scanning electron microscopy) and structure (by Fourier transform infrared spectroscopy and grazing incidence X-ray diffraction), the corrosion resistance of the RF-MS coated Mg-0.8Ca substrates was electrochemically tested (in synthetic biological media with different degrees of biomimicry), and their cytocompatibility was assessed in osteoblast and fibroblast cell cultures. By collective assessment, the most promising performances, in terms of mass loss (similar to 7% after 12 days), hydrogen release rate (similar to 6 mL/cm(2) after 12 days), electrochemical corrosion parameters and cytocompatibility, were obtained for the crystalline HA coating.
40. Influence of the synthesis parameters on the transport properties of Mg2Si0.4Sn0.6 solid solutions produced by melting and spark plasma sintering
Authors: Assahsahi, I; Popescu, B; Enculescu, M; Galatanu, M; Galca, AC; El Bouayadi, R; Zejli, D; Galatanu, A

Published: APR 2022, JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS, 163, DOI: 10.1016/j.jpcs.2021.110561

In this work, the influence of the preparation route on the structural, morphological, and thermoelectric properties of the Mg2Si0.4Sn0.6 solid solutions is investigated. The synthesis based on melting the constituent elements in a closed graphite crucible followed by spark plasma sintering allows mixing elements with a large difference of their melting temperatures and a good control of sample stoichiometry. The optimized synthesis route is validated by the doped V and Sb samples, which yield good thermoelectric performance. The n-type doping leads to two orders of magnitude increase of the carrier concentration, and thus a subsequent increase of the electrical conductivity, which, in turn, augments greatly the power factor of the Mg1.98V0.02Si0.385Sn0.6Sb0.015 to 42.61 x10(-4) Wm(-1)K 2 at 650K. Although doping slightly enlarges the thermal conductivity, a peak value of the figure of merit ZT similar to 1.15 is obtained at 723K, which is 20 times higher than the ZT of un-doped material.

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