1. Synthesis of complex concentrated nanoparticles by Ultrasonic Spray Pyrolysis and lyophilisationLidija Simić, Srečko Stopić, Bernd Friedrich, Matej Zadravec, Žiga Jelen, Rajko Bobovnik, Ivan Anžel, Rebeka Rudolf, 2022, izvirni znanstveni članek Opis: The development of new multicomponent nanoparticles is gaining increasing importance
due to their specific functional properties, i.e., synthesised new complex concentrated nanoparticles
(CCNPs) in the form of powder using ultrasonic spray pyrolysis (USP) and lyophilisation from the
initial cast Ag20Pd20Pt20Cu20Ni20 alloy, which was in the function of the material after its catalytic
abilities had been exhausted. Hydrometallurgical treatment was used to dissolve the cast alloy,
from which the USP precursor was prepared. As a consequence of the incomplete dissolution of
the cast alloy and the formation of Pt and Ni complexes, it was found that the complete recycling
of the alloy is not possible. A microstructural examination of the synthesised CCNPs showed that
round and mostly spherical (not 100%) nanoparticles were formed, with an average diameter of
200 nm. Research has shown that CCNPs belong to the group with medium entropy characteristics.
A mechanism for the formation of CCNPs is proposed, based on the thermochemical analysis of
element reduction with the help of H2 and based on the mixing enthalpy of binary systems. Ključne besede: complex concentrated nanoparticles, ultrasonic spray pyrolysis, lyophilisation, characterization, formation mechanism Objavljeno v DKUM: 24.03.2025; Ogledov: 0; Prenosov: 2
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2. Synthesis of Ni/Y2O3 nanocomposite through USP and lyophilisation for possible use as coatingTilen Švarc, Srečko Stopić, Žiga Jelen, Matej Zadravec, Bernd Friedrich, Rebeka Rudolf, 2022, izvirni znanstveni članek Opis: The Ni/Y2O3 catalyst showed high catalytic activity. Based on this, the aim of this study
was to create Ni/Y2O3 nanocomposites powder with two innovative technologies, Ultrasonic Spray
Pyrolysis (USP) and lyophilisation. In the USP process, thermal decomposition of the generated
aerosols in an N2/H2 reduction atmosphere caused a complete decomposition of the nickel (II) nitrate
to elemental Ni, which became trapped on the formed Y2O3 nanoparticles. The Ni/Y2O3 nanocomposite particles were captured via gas washing in an aqueous solution of polyvinylpyrrolidone (PVP)
in collection bottles. PVP was chosen for its ability to stabilise nano-suspensions and as an effective
cryoprotectant. Consequently, there was no loss or agglomeration of Ni/Y2O3 nanocomposite material during the lyophilisation process. The Ni/Y2O3 nanocomposite powder was analysed using
ICP-MS, SEM-EDX, and XPS, which showed the impact of different precursor concentrations on the
final Ni/Y2O3 nanocomposite particle composition. In a final step, highly concentrated Ni/Y2O3
nanocomposite ink (Ni/Y2O3 > 0.140 g/mL) and test coatings from this ink were prepared by applying them on a white matte photo paper sheet. The reflection curve of the prepared Ni/Y2O3
nanocomposite coating showed a local maximum at 440 nm with a value of 39% reflection. Given that
Ni is located on the surface of the Ni/Y2O3 nanocomposite in the elemental state and according to the
identified properties, tests of the catalytic properties of this coating will be performed in the future. Ključne besede: Ultrasonic Spray Pyrolysis (USP), lyophilisation, Ni/Y2O3 nanocomposite, characterisation, coatings Objavljeno v DKUM: 20.03.2025; Ogledov: 0; Prenosov: 6
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3. Recovery study of gold nanoparticle markers from lateral flow immunoassaysTilen Švarc, Peter Majerič, Darja Feizpour, Žiga Jelen, Matej Zadravec, Timi Gomboc, Rebeka Rudolf, 2023, izvirni znanstveni članek Opis: Lateral flow immunoassays (LFIAs) are a simple diagnostic device used to detect targeted analytes. Wasted and unused rapid antigen lateral flow immunoassays represent mass waste that needs to be broken down and recycled into new material components. The aim of this study was to recover gold nanoparticles that are used as markers in lateral flow immunoassays. For this purpose, a dissolution process with aqua regia was utilised, where gold nanoparticles were released from the lateral flow immunoassay conjugate pads. The obtained solution was then concentrated further with gold chloride salt (HAuCl4) so that it could be used for the synthesis of new gold nanoparticles in the process of ultrasonic spray pyrolysis (USP). Various characterisation methods including scanning electron microscopy, transmission electron microscopy, ultraviolet-visible spectroscopy and optical emission spectrometry with inductively coupled plasma were used during this study. The results of this study showed that the recovery of gold nanoparticles from lateral flow immunoassays is possible, and the newly synthesised gold nanoparticles represent the possibility for incorporation into new products. Ključne besede: gold nanoparticles, recovery, LFIA, ultrasonic spray pyrolysis, characterisation Objavljeno v DKUM: 09.02.2024; Ogledov: 358; Prenosov: 25
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4. Polyvinylpyrrolidone-stabilised gold nanoparticle coatings inhibit blood protein adsorptionHanuma Reddy Tiyyagura, Matej Bračič, Rebeka Rudolf, 2024, izvirni znanstveni članek Opis: In this work, the ability of polyvinylpyrrolidone (PVP)-stabilised gold nanoparticle (AuNP) coatings to inhibit blood protein adsorption was evaluated by studying timeresolved solid–liquid interactions of the coatings with the model blood protein bovine serum albumin (BSA). Inhibiting unspecific blood protein adsorption is of crucial importance for blood-contacting implant devices, e.g. vascular grafts, stents, artificial joints, and others, as a preventive strategy for bacterial biofilm formation. A quartz crystal microbalance was used in this work to coat the AuNPs on piezoelectric sensors and to follow time-resolved solid–liquid interactions with the proteins. The AuNP coatings were evaluated for their wettability by contact angle measurements, their surface morphology by lightand atomic force microscopy, and their chemical composition by energy-dispersive X-ray spectroscopy. Results revealed a homogeneous distribution of AuNPs on the sensor surface with a dry mass coverage of 3.37 ± 1.46 µg/cm2 and a contact angle of 25.2 ± 1.1°. Solid–liquid interaction studies by quartz crystal microbalance showed a high repellence of BSA from the PVP-stabilised AuNP coatings and the importance of the PVP in the mechanism of repellence. Furthermore, the conformation of the polymer on the coatings as well as its viscoelastic properties were revealed. Finally, the activated partial thrombin time test and fibrinogen adsorption studies revealed that the AuNPs do not accelerate blood coagulation and can partially inhibit the adhesion of fibrinogen, which is a crucial factor in the common blood coagulation cascade. Such AuNPs have the potential to be used in blood-contact medical applications. Ključne besede: gold nanoparticles, ultrasonic spray pyrolysis, haemocompatibility, protein adsorption, quartz crystal microbalance Objavljeno v DKUM: 30.01.2024; Ogledov: 377; Prenosov: 33
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5. Melting point of dried gold nanoparticles prepared with ultrasonic spray pyrolysis and lyophilisationŽiga Jelen, Marcin Krajewski, Franc Zupanič, Peter Majerič, Tilen Švarc, Ivan Anžel, Jernej Ekar, Sz-Chian Liou, Jerzy Kubacki, Mateusz Tokarczyk, Rebeka Rudolf, 2023, izvirni znanstveni članek Opis: A coupled process of ultrasonic spray pyrolysis and lyophilisation was used for the synthesis of dried gold nanoparticles. Two methods were applied for determining their melting temperature: uniaxial microcompression and differential scanning calorimetry (DSC) analysis. Uniaxial microcompression resulted in sintering of the dried gold nanoparticles at room temperature with an activation energy of 26–32.5 J/g, which made it impossible to evaluate their melting point. Using DSC, the melting point of the dried gold nanoparticles was measured to be around 1064.3°C, which is close to pure gold. The reason for the absence of a melting point depression in dried gold nanoparticles was their exothermic sintering between 712 and 908.1°C. Ključne besede: gold nanoparticles, melting point, ultrasonic spray pyrolysis, characterisation Objavljeno v DKUM: 08.12.2023; Ogledov: 448; Prenosov: 32
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6. Study of gold nanoparticles conjugated with SARS-CoV-2 S1 spike protein fragmentsŽiga Jelen, Janez Kovač, Rebeka Rudolf, 2023, izvirni znanstveni članek Opis: This study reports on the successful conjugation of SARS-CoV-2 S1 spike protein fragments with gold nanoparticles (AuNPs) that were synthesised with Ultrasonic Spray Pyrolysis (USP). This method enables the continuous synthesis of AuNPs with a high degree of purity, round shapes, and the formation of a surface that allows various modifications. The conjugation mechanism of USP synthesized AuNPs with SARS-CoV-2 S1 spike protein fragments was investigated. A gel electrophoresis experiment confirmed the successful conjugation of AuNPs with SARS-CoV-2 S1 fragments indirectly. X-ray Photoelectron Spectroscopy (XPS) analysis confirmed the presence of characteristic O1s and N1s peaks, which indicated that specific binding between AuNPs and SARS-CoV-2 S1 spike protein fragments takes place via a peptide bond formed with the citrate stabiliser. This bond is coordinated to the AuNP’s surface and the N-terminals of the protein, with the conjugate displaying the expected response within a prototype LFIA test. This study will help in better understanding the behaviour of AuNPs synthesised with USP and their potential use as sensors in colorimetric or electrochemical sensors and LFIA tests. Ključne besede: gold nanoparticles, ultrasonic spray pyrolysis, conjugation, SARS-CoV-2 S1, characterisation Objavljeno v DKUM: 07.12.2023; Ogledov: 416; Prenosov: 26
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7. Physicochemical properties of gold nanoparticles for skin care creamsPeter Majerič, Zorana Jović, Tilen Švarc, Žiga Jelen, Andrej Horvat, Djuro Koruga, Rebeka Rudolf, 2023, izvirni znanstveni članek Opis: Gold nanoparticles (AuNPs) have now been used in skin care creams for several years, with marketed anti-aging, moisturizing, and regenerative properties. Information on the harmful effects of these nanoparticles is lacking, a concern for the use of AuNPs as cosmetic ingredients. Testing AuNPs without the medium of a cosmetic product is a typical method for obtaining this information, which is mainly dependent on their size, shape, surface charge, and dose. As these properties depend on the surrounding medium, nanoparticles should be characterized in a skin cream without extraction from the cream’s complex medium as it may alter their physicochemical properties. The current study compares the sizes, morphology, and surface changes of produced dried AuNPs with a polyvinylpyrrolidone (PVP) stabilizer and AuNPs embedded in a cosmetic cream using a variety of characterization techniques (TEM, SEM, DLS, zeta potential, BET, UV–vis). The results show no observable differences in their shapes and sizes (spherical and irregular, average size of 28 nm) while their surface charges changed in the cream, indicating no major modification of their primary sizes, morphology, and the corresponding functional properties. They were present as individually dispersed nanoparticles and as groups or clusters of physically separated primary nanoparticles in both dry form and cream medium, showing suitable stability. Examination of AuNPs in a cosmetic cream is challenging due to the required conditions of various characterization techniques but necessary for obtaining a clear understanding of the AuNPs’ properties in cosmetic products as the surrounding medium is a critical factor for determining their beneficial or harmful effects in cosmetic products. Ključne besede: gold nanoparticles, ultrasonic spray pyrolysis, freeze drying, characterization, creams Objavljeno v DKUM: 19.04.2023; Ogledov: 769; Prenosov: 79
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8. Formation of bimetallic Fe/Au submicron particles with Ultrasonic Spray PyrolysisPeter Majerič, Darja Feizpour, Bernd Friedrich, Rebeka Rudolf, 2018, izvirni znanstveni članek Ključne besede: ultrasonic spray pyrolysis, precursor salts, formation mechanism, nanoparticle structure, Fe oxides, Au Objavljeno v DKUM: 19.04.2018; Ogledov: 1660; Prenosov: 366
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9. Structure and formation model of Ag/TiO2 and Au/TiO2 nanoparticles synthesized through Ultrasonic Spray PyrolysisAlkan Gözde, Rebeka Rudolf, Jelena Bogovic, Darja Feizpour, Bernd Friedrich, 2017, izvirni znanstveni članek Ključne besede: ultrasonic spray pyrolysis, core shell nanostructure, formation mechanism, TiO2, Ag, Au Objavljeno v DKUM: 26.09.2017; Ogledov: 1469; Prenosov: 443
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10. Morphology, aggregation properties, cytocompatibility and anti-inflammatory potential of citrate-stabilized AuNPs prepared by modular Ultrasonic Spray PyrolysisRebeka Rudolf, Peter Majerič, Sergej Tomić, Mohammed Shariq, Urban Ferčec, Bojan Budič, Bernd Friedrich, Dragana Vučević, Miodrag Čolić, 2017, izvirni znanstveni članek Opis: Ultrasonic Spray Pyrolysis (USP) possesses a great potential for production of higher quantities of gold nanoparticles (AuNPs), thus overcoming the problem of batch-to-batch variations in their properties. Recently, we demonstrated that USP with an additional evaporation chamber (modular USP) led to a better size control of AuNPs. However, their morphology, stability, toxicity, and immunomodulatory properties have not been investigated completely. Here, two types of spherical AuNPs were produced by using different USP parameters, followed by their stabilization in Na-citrate solution. No significant changes in their size, agglomeration, and -potential occurred 3 months after their initial production in citrate solution. However, the conditioning of AuNPs in serum-containing cell culture media for 24 h induced an increase in the AuNPs’ hydrodynamic size and a red shift in their Surface Plasmon Resonance, pointing to their instability in biological media. Cytocompatibility tests showed that the produced AuNPs were internalized by L929 cells and primary human monocytes and were not cytotoxic at the concentrations lower than 200 μg/mL, but they exhibited antiproliferative and anti-inflammatory effects, respectively. AuNPs reduced the percentage of CD14+CD16+ but not CD14lowCD16+ monocytes in vitro and reduced the expression of CD86, HLA-DR, TNF-α, and IL-12/IL-23 by these cells. These results indicate that the anti-inflammatory effects of citrate-capped AuNPs produced by modular USP could be beneficial for their application in the treatment of inflammatory conditions. Ključne besede: Ultrasonic Spray Pyrolysis, gold nanoparticles, plasmon resonance, monocytes, antiinflammatory effects Objavljeno v DKUM: 14.06.2017; Ogledov: 1594; Prenosov: 420
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