National Institute Of Materials Physics - Romania

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51. Electro-active properties of nanostructured films of cytosine and guanine nucleobases
Authors: Socol, M; Trupina, L; Galca, AC; Chirila, C; Stan, GE; Vlaicu, AM; Stanciu, AE; Boni, AG; Botea, M; Stanculescu, A; Pintilie, L; Borca, B

Published: OCT 8 2021, NANOTECHNOLOGY, 32, DOI: 10.1088/1361-6528/ac10e4

The discovery of multifunctional properties related to electro-activity of organic systems of biomolecules is important for a variety of applications, especially for devices in the realm of biocompatible sensors and/or bioactuators. A further step towards such applications is to prepare thin films with the required properties. Here, the investigation is focused on the characterization of films of guanine and cytosine nucleobases, prepared by thermal evaporation-an industrial accessible deposition technique. The cytosine films have an orthorhombic non-centrosymmetric structure and grow in two interconnected nanostructured fractal patterns, of nearly equal proportion. Piezoresponse force microscopy images acquired at room temperature on the cytosine films display large zones with antiparallel alignment of the vertical components of the polarization vector. Guanine films have a dense nano-grained morphology. Our studies reveal electrical polarization switching effects which can be related to ferroelectricity in the films of guanine molecules. Characteristic ferroelectric polarization-electric-field hysteresis loops showing large electrical polarization are observed at low temperatures up to 200 K. Above this temperature, the guanine films have a preponderant paraelectric phase containing residual or locally induced nano-scopic ferroelectric domains, as observed by piezoresponse force microscopy at room temperature.
52. Physico-chemical properties of two anhydrous azathioprine forms and their interaction with typical pharmaceutical excipients: highlighting new findings in drug formulation development
Authors: Barbatu, A; Lungan, MA; Toulbe, N; Smaranda, I; Daescu, M; Baibarac, M; Manta, CM

Published: OCT 3 2021, DRUG DEVELOPMENT AND INDUSTRIAL PHARMACY, 47, DOI: 10.1080/03639045.2022.2032131

The physico-chemical properties of two anhydrous AZA forms and their interaction with typical pharmaceutical excipients were assessed by applying various methods (such as PXRD, HPLC, TG/DSC, IR, Raman, PL or UV-Vis) in order to highlight new directions for drug formulation. The stability assessment of AZA anhydrous forms I and II was performed in order to determine the risk of degradation of the active ingredient by accidental exposure to nonstandard conditions in the industrial environment, under different storage, transport or processing conditions. The benefits of form II include increased resistance to chemical degradation over a wide range of pH, but further control of storage and processing conditions is necessary to avoid polymorphic transformation into form I. The solubility assessment on the AZA solid forms in different environments that simulate the conditions of the gastrointestinal tract has the advantage of a significantly increased solubility of form II compared with the commercial form I due to the modification of the crystalline structure. In the case of capsules compared to AZA form I or II as powder, an improvement in their solubility was observed, promoted by the presence of one or more excipients in the formulation mixture.
53. Composite Drug Delivery System Based on Amorphous Calcium Phosphate-Chitosan: An Efficient Antimicrobial Platform for Extended Release of Tetracycline
Authors: Visan, AI; Ristoscu, C; Popescu-Pelin, G; Sopronyi, M; Matei, CE; Socol, G; Chifiriuc, MC; Bleotu, C; Grossin, D; Brouillet, F; Le Grill, S; Bertrand, G; Zgura, I; Cristescu, R; Mihailescu, IN

Published: OCT 2021, PHARMACEUTICS, 13, DOI: 10.3390/pharmaceutics13101659

One major warning emerging during the first worldwide combat against healthcare-associated infections concerns the key role of the surface in the storage and transfer of the virus. Our study is based on the laser coating of surfaces with an inorganic/organic composite mixture of amorphous calcium phosphate-chitosan-tetracycline that is able to fight against infectious agents, but also capable of preserving its activity for a prolonged time, up to several days. The extended release in simulated fluids of the composite mixture containing the drug (tetracycline) was demonstrated by mass loss and UV-VIS investigations. The drug release profile from our composite coatings proceeds via two stages: an initial burst release (during the first hours), followed by a slower evolution active for the next 72 h, and probably more. Optimized coatings strongly inhibit the growth of tested bacteria (Enterococcus faecalis and Escherichia coli), while the drug incorporation has no impact on the in vitro composite's cytotoxicity, the coatings proving an excellent biocompatibility sustaining the normal development of MG63 bone-like cells. One may, therefore, consider that the proposed coatings' composition can open the prospective of a new generation of antimicrobial coatings for implants, but also for nosocomial and other large area contamination prevention.
54. A nanoscale continuous transition from the monoclinic to ferroelectric orthorhombic phase inside HfO2 nanocrystals stabilized by HfO2 capping and self-controlled Ge doping
Authors: Palade, C; Lepadatu, AM; Slav, A; Cojocaru, O; Iuga, A; Maraloiu, VA; Moldovan, A; Dinescu, M; Teodorescu, VS; Stoica, T; Ciurea, ML

Published: SEP 28 2021, JOURNAL OF MATERIALS CHEMISTRY C, 9, 12366, DOI: 10.1039/d1tc02921e

Orthorhombic HfO2 exhibits nanoscale ferroelectricity that opens the perspective of ultra-scalable CMOS integration of ferroelectric memories. However, many aspects of the metastable orthorhombic crystallization mechanisms still need to be elucidated and new fabrication methods are of high interest. In this paper, the atomically resolved crystal structure of HfO2 is a 3-layer structure with a Ge-rich HfO2 intermediate layer capped by a top (cap) HfO2 layer and cladded by a bottom HfO2 layer. There is a continuity of crystal growth from the top and bottom HfO2 layers into the intermediate layer. A spatial transition from a monoclinic phase to an orthorhombic phase was revealed within a region of a few atomic layers at the interface between capped and intermediate HfO2 layers. This result suggests the mechanism of orthorhombic and monoclinic phase formation by a martensitic-like transformation of the initially grown tetragonal phase. The sample fabrication method we used involved magnetron sputtering deposition of the 3-layer structures, i.e. a stack of top HfO2/Ge-rich HfO2 intermediate/bottom HfO2 layers, followed by rapid thermal annealing. It results in self-optimized orthorhombic crystallization of HfO2 by Ge nanoparticle segregation in the intermediate layer. The ferroelectric effects are revealed by polarization-voltage hysteresis loops and piezoresponse force microscopy measurements. The atomistic computations performed by using the density functional theory support the experimental results by showing that the Ge doping of HfO2 leads to orthorhombic phase stabilization and increased Berry phase polarization.
55. Synthesis and Characterization of Cu2ZnSnS4 Thin Films Obtained by Combined Magnetron Sputtering and Pulsed Laser Deposition
Authors: Zaki, MY; Sava, F; Buruiana, AT; Simandan, ID; Becherescu, N; Galca, AC; Mihai, C; Velea, A

Published: SEP 2021, NANOMATERIALS, 11, DOI: 10.3390/nano11092403

Cu2ZnSnS4 (CZTS) is a complex quaternary material, and obtaining a single-phase CZTS with no secondary phases is known to be challenging and dependent on the production technique. This work involves the synthesis and characterization of CZTS absorber layers for solar cells. Thin films were deposited on Si and glass substrates by a combined magnetron sputtering (MS) and pulsed laser deposition (PLD) hybrid system, followed by annealing without and with sulfur powder at 500 degrees C under argon (Ar) flow. Three different Cu2S, SnS2, and ZnS targets were used each time, employing a different target for PLD and the two others for MS. The effect of the different target arrangements and the role of annealing and/or sulfurization treatment were investigated. The characterization of the absorber films was performed by grazing incidence X-ray diffraction (GIXRD), X-ray reflectometry (XRR), Raman spectroscopy, scanning electron microscopy, and regular transmission spectroscopy. The film with ZnS deposited by PLD and SnS2 and Cu2S by MS was found to be the best for obtaining a single CZTS phase, with uniform surface morphology, a nearly stoichiometric composition, and an optimal band gap of 1.40 eV. These results show that a new method that combines the advantages of both MS and PLD techniques was successfully used to obtain single-phase Cu2ZnSnS4 films for solar cell applications.
56. Hydrocarbons detection using surface plasmon resonance with As2S3 thin film waveguide
Authors: Baschir, L; Miclos, S; Savastru, D; Simandan, ID; Popescu, AA

Published: SEP 2021, CHALCOGENIDE LETTERS, 18, 540, DOI:

Surface plasmon resonance containing amorphous As2S3 film is proposed as a chemical sensor to highlight several liquid hydrocarbons. Method is label-free and is based on detection of small changes in the refractive index. As2S3 operates as plasmonic waveguide which confines the probing beam to the interface with liquid hydrocarbons. The method can easily distinguish hydrocarbons with very close refractive indices. The film thicknesses were optimized to obtain the best sensitivity and resolving power Minimum reflectance of SPR less than 1 % was found for optimal calculated film thicknesses, the sensitivity to the refractive index changes being 2.10(-5).
57. The Effect of the Deposition Method on the Structural and Optical Properties of ZnS Thin Films
Authors: Simandan, ID; Sava, F; Buruiana, AT; Burducea, I; Becherescu, N; Mihai, C; Velea, A; Galca, AC

Published: SEP 2021, COATINGS, 11, DOI: 10.3390/coatings11091064

ZnS is a wide band gap material which was proposed as a possible candidate to replace CdS as a buffer layer in solar cells. However, the structural and optical properties are influenced by the deposition method. ZnS thin films were prepared using magnetron sputtering (MS), pulsed laser deposition (PLD), and a combined deposition technique that uses the same bulk target for sputtering and PLD at the same time, named MSPLD. The compositional, structural, and optical properties of the as-deposited and annealed films were inferred from Rutherford backscattering spectrometry, X-ray diffraction, X-ray reflectometry, Raman spectroscopy, and spectroscopic ellipsometry. PLD leads to the best stoichiometric transfer from target to substrate, MS makes fully amorphous films, whereas MSPLD facilitates obtaining the densest films. The study reveals that the band gap is only slightly influenced by the deposition method, or by annealing, which is encouraging for photovoltaic applications. However, sulphur vacancies contribute to lowering the bandgap and therefore should be controlled. Moreover, the results add valuable information towards the understanding of ZnS polymorphism. The combined MSPLD method offers several advantages such as an increased deposition rate and the possibility to tune the optical properties of the obtained thin films.
58. Comparative investigation of structural, EPR, optical and photoluminescence properties of nanostructured LaPO4:Ce/RE/Me and LaPO4:Yb/Er phosphors prepared by co-precipitation method
Authors: AitMellal, O; Oufni, L; Messous, MY; Trandafir, MM; Chirica, IM; Florea, M; Neatu, S; Rostas, AM; Secu, M; Neatu, F

Published: SEP 2021, JOURNAL OF SOLID STATE CHEMISTRY, 301, DOI: 10.1016/j.jssc.2021.122310

In this work, the structural, thermal, vibrational, morphological, magnetic and optical properties of LaPO4:Ce/RE/Me (RE=Nd3+, Tb3+; Me-Cr3+, Mn2+) and LaPO4:Yb3+/Er3+ phosphors prepared by the co-precipitation method are presented. The obtained materials crystallized in monoclinic structure with the P2(1)/n space group and the particles were of nanorod shape with about 200 nm in length and the diameter approximately 19 nm. The presence of dopant ions was confirmed by both electron paramagnetic resonance (EPR) and UV-visible spectroscopies. In addition, the down-conversion (DC) and up-conversion (UC) of the LaPO4 nanophosphors via the 275 and 980 nm excitations, respectively, were considered, and a wide range of electronic transitions was observed. Based on the photoluminescence (PL) spectra, there is an efficient energy transfer (ET) process from Ce3+ donors to Nd3+ and Tb3+ acceptors, and the computed ET efficiency was 70% and 88%, respectively. The Ce3+/Cr3+ and Ce3+/Mn2+ doped LaPO4 showed weak far-red and green luminescence with much smaller ET efficiency of about 3.7 and 0.4%, respectively. LaPO4:Yb3+/Er3+ showed UC luminescence under the 980 nm laser radiation, and the resulted red and green light was attributed to the Er3+ transitions.
59. Silicon Metalens Fabrication from Electron Beam to UV-Nanoimprint Lithography
Authors: Baracu, AM; Avram, MA; Breazu, C; Bunea, MC; Socol, M; Stanculescu, A; Matei, E; Thrane, PCV; Dirdal, CA; Dinescu, A; Rasoga, O

Published: SEP 2021, NANOMATERIALS, 11, DOI: 10.3390/nano11092329

This study presents the design and manufacture of metasurface lenses optimized for focusing light with 1.55 mu m wavelength. The lenses are fabricated on silicon substrates using electron beam lithography, ultraviolet-nanoimprint lithography and cryogenic deep reactive-ion etching techniques. The designed metasurface makes use of the geometrical phase principle and consists of rectangular pillars with target dimensions of height h = 1200 nm, width w = 230 nm, length l = 354 nm and periodicity p = 835 nm. The simulated efficiency of the lens is 60%, while the master lenses obtained by using electron beam lithography are found to have an efficiency of 45%. The lenses subsequently fabricated via nanoimprint are characterized by an efficiency of 6%; the low efficiency is mainly attributed to the rounding of the rectangular nanostructures during the pattern transfer processes from the resist to silicon due to the presence of a thicker residual layer.
60. Design of highly transparent conductive optical coatings optimized for oblique angle light incidence
Authors: Nedelcu, N; Chiroiu, V; Munteanu, L; Girip, I; Rugina, C; Lorinczi, A; Matei, E; Sobetkii, A

Published: AUG 2021, APPLIED PHYSICS A-MATERIALS SCIENCE & PROCESSING, 127, DOI: 10.1007/s00339-021-04726-z

In this paper, three deposition techniques are combined to create a window material with high average transmission at oblique angles of incidence. Spectrophotometry and ellipsometry measurements, respectively, yield the optical constants n and k. In contrast with other analyses on the subject, a high average transmission, higher than 91% in the 450-900 nm spectral range, is obtained at incident angles of 20-25 degrees. The refractive index and extinction coefficient are determined by the Swanepoel method. The iterative optimization performed using the OpenFilters software leads to an antireflection (AR) multilayer with low reflection and high transmission. The surface quality of the films was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM), which revealed compact, continuous, and smooth films.

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