Search Results (38)

Thermoplasmonic heat generation by silver (Ag) nanoparticles can harness visible light to efficiently produce localized heating. Flame spray pyrolysis (FSP) is a powerful one-step synthesis technology for fabricating plasmonic Ag-based nanostructures. In the present study, we employed FSP to engineer core@shell Ag@SiO₂ nanoparticles coated with an ultrathin (1–2 nm) silica (SiO₂) nanolayer in a single step in tandem with their deposition as films onto solid substrates. Accordingly, we engineered a library of Ag@SiO₂ nanofilms with precisely controlled thicknesses in the range of 1–23 μm. A systematic study of the thermoplasmonic heat-generation efficiency (ΔT) of the films under visible-light irradiation (LED, λ = 405 nm) revealed that the films’ compactness and thickness are key parameters governing the heat-generation efficiency and thermal response rate. Moreover, we show that the substrate type can also play a key role; Ag@SiO₂ films on glass-fiber filters (PGFFs) enabled faster temperature increase (dT/dt) and a higher maximum temperature gain (ΔT_max) compared with Ag@SiO₂ films on glass substrates (PGSs). The photothermal conversion efficiencies were approximately 60%, with the highest efficiency (η = 65%) observed in the thinner impinged film. This study demonstrates that FSP-derived Ag@SiO₂ nanofilms provide a versatile and scalable platform for thermoplasmonic heat generation applications with significant industrial potential. Full article

In this work, three catalysts, TiO₂, WO₃ and TiO₂/WO₃, have been synthesized through flame spray pyrolysis synthesis (FSP) and have been tested for CO₂ photoreduction. The catalysts were fully characterized by XRD, DRS UV–Vis, N₂ physisorption and SEM. Experimental tests were performed in a one-of-a-kind high-pressure reactor at 18 bar. TiO₂ P25 was used as a benchmark to compare the productivities of the newly synthetized catalysts. The two single oxides showed comparable productivities, both slightly lower than the P25 reference value (ca. 17 mol/kg_cat·h). The mixed oxide, TiO₂/WO₃, instead showed an impressive productivity of formic acid with 36 mol/kg_cat·h, which is around 2.5 times higher than both of the single oxides alone. The formation of a type-II heterojunction has been confirmed through DRS analysis. The remarkable productivity demonstrates how FSP synthesis can be a crucial tool to obtain highly active and stable photocatalysts. This approach has already been successfully scaled up for the industrial production of various catalysts, showcasing its versatility and efficiency. Full article

Nanocrystalline TiO₂ is a perspective semiconductor gas-sensing material due to its long-term stability of performance, but it is limited in application because of high electrical resistance. In this paper, a gas-sensing nanocomposite material with p-p heterojunction is introduced based on p-conducting Cr-doped TiO₂ in combination with p-conducting Cr₂O₃. Materials were synthesized via a single-step flame spray pyrolysis (FSP) technique and comprehensively studied by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) specific surface area analysis, transition electron microscopy (TEM), energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR), and Raman spectroscopy. Gas sensor performance in direct current (DC) mode was studied toward a number of gasses (H₂, CO, CH₄, NO₂, H₂S, NH₃) as well as volatile organic compounds (VOCs) (acetone, methanol, and formaldehyde) in dry and humid conditions. The long-term stability of the obtained materials’ gas sensor performance was evaluated alongside with an ex situ study of structural evolution. High sensitivity toward oxygenated VOCs and a lower detection limit below ppm level with a limited influence of humidity were shown. The long-term gas sensor performance stability of the obtained materials and its connection to the defect structure of doped TiO₂ is demonstrated. Full article

Several Cu and Ni-based catalysts were synthetized over Ce-based supports, either pure or mixed with different amounts of alumina (1:2 and 1:3 mol/mol). Different metal loadings (10–40 wt%) and preparation methods (wet impregnation, co-precipitation, and flame-spray pyrolysis—FSP) were compared for the oxidative steam reforming of methanol. Characterization of the catalysts has been performed, e.g., through XRD, BET, XPS, TPR, SEM, and EDX analyses. All the catalysts have been tested in a bench-scale continuous setup. The hydrogen yield and methanol conversion obtained have been correlated with the operating conditions, metal content, crystallinity of the catalyst particles, total surface area, and with the interaction of the metal with the support. A Cu loading of 20% wt/wt was optimal, while the presence of alumina was not beneficial, decreasing catalyst activity at low temperatures compared with catalysts supported on pure CeO₂. Ni-based catalysts were a possible alternative, but the activity towards the methanation reaction at relatively high temperatures decreased inevitably the hydrogen yield. Durability and deactivation tests showed that the best-performing catalyst, 20% wt. Cu/CeO₂ prepared through coprecipitation was stable for a long period of time. Full methanol conversion was achieved at 280 °C, and the highest yield of H₂ was ca. 80% at 340 °C, higher than the literature data. Full article

Lithium tantalate (LiTaO₃) perovskite finds wide use in pyroelectric detectors, optical waveguides and piezoelectric transducers, stemming from its good mechanical and chemical stability and optical transparency. Herein, we present a method for synthesis of LiTaO₃ nanoparticles using a scalable Flame Spray Pyrolysis (FSP) technology, that allows the formation of LiTaO₃ nanomaterials in a single step. Raman, XRD and TEM studies allow for comprehension of the formation mechanism of the LiTaO₃ nanophases, with particular emphasis on the penetration of Li atoms into the Ta-oxide lattice. We show that, control of the High-Temperature Particle Residence Time (HTPRT) in the FSP flame, is the key-parameter that allows successful penetration of the -otherwise amorphous- Li phase into the Ta₂O₅ nanophase. In this way, via control of the HTPRT in the FSP process, we synthesized a series of nanostructured LiTaO₃ particles of varying phase composition from {amorphous Li/Ta₂O₅/LiTaO₃} to {pure LiTaO₃, 15–25 nm}. Finally, the photophysical activity of the FSP-made LiTaO₃ was validated for photocatalytic H₂ production from H₂O. These data are discussed in conjunction with the role of the phase composition of the LiTaO₃ nanoparticles. More generally, the present work allows a better understanding of the mechanism of ABO₃ perovskite formation that requires the incorporation of two cations, A and B, into the nanolattice. Full article

Engineering of oxygen vacancies (Vo) in nanomaterials allows diligent control of their physicochemical properties. SrTiO₃ possesses the typical ABO₃ structure and has attracted considerable attention among the titanates due to its chemical stability and its high conduction band energy. This has resulted in its extensive use in photocatalytic energy-related processes, among others. Herein, we introduce the use of Flame Spray Pyrolysis (FSP); an industrial and scalable process to produce Vo-rich SrTiO₃ perovskites. We present two types of Anoxic Flame Spray Pyrolysis (A-FSP) technologies using CH₄ gas as a reducing source: Radial A-FSP (RA-FSP); and Axial A-FSP (AA-FSP). These are used for the control engineering of oxygen vacancies in the SrTiO_3-x nanolattice. Based on X-ray photoelectron spectroscopy, Raman and thermogravimetry-differential thermal analysis, we discuss the role and the amount of the Vos in the so-produced nano-SrTiO_3-x, correlating the properties of the nanolattice and energy-band structure of the SrTiO_3-x. The present work further corroborates the versatility of FSP as a synthetic process and the potential future application of this process to engineer photocatalysts with oxygen vacancies in quantities that can be measured in kilograms. Full article

Flame spray pyrolysis (FSP) is an industrially scalable technology that enables the engineering of a wide range of metal-based nanomaterials with tailored properties nanoparticles. In the present review, we discuss the recent state-of-the-art advances in FSP technology with regard to nanostructure engineering as well as the FSP reactor setup designs. The challenges of in situ incorporation of nanoparticles into complex functional arrays are reviewed, underscoring FSP’s transformative potential in next-generation nanodevice fabrication. Key areas of focus include the integration of FSP into the technology readiness level (TRL) for nanomaterials production, the FSP process design, and recent advancements in nanodevice development. With a comprehensive overview of engineering methodologies such as the oxygen-deficient process, double-nozzle configuration, and in situ coatings deposition, this review charts the trajectory of FSP from its foundational roots to its contemporary applications in intricate nanostructure and nanodevice synthesis. Full article

Cu₂O is among the most promising photocatalysts for CO₂ reduction, however its photocorrosion remains a standalone challenge. Herein, we present an in situ study of the release of Cu ions from Cu₂O nanocatalysts under photocatalytic conditions in the presence of HCO₃ as a catalytic substrate in H₂O. The Cu-oxide nanomaterials were produced by Flame Spray Pyrolysis (FSP) technology. Using Electron Paramagnetic Resonance (EPR) spectroscopy in tandem with analytical Anodic Stripping Voltammetry (ASV), we monitored in situ the Cu²⁺ atom release from the Cu₂O nanoparticles in comparison with CuO nanoparticles under photocatalytic conditions. Our quantitative, kinetic data show that light has detrimental effect on the photocorrosion of Cu₂O and ensuing Cu²⁺ ion release in the H₂O solution, up to 15.7% of its mass. EPR reveals that HCO₃ acts as a ligand of the Cu²⁺ ions, promoting the liberation of {HCO₃-Cu} complexes in solution from Cu₂O, up to 27% of its mass. HCO₃ alone exerted a marginal effect. XRD data show that under prolonged irradiation, part of Cu²⁺ ions can reprecipitate on the Cu₂O surface, creating a passivating CuO layer that stabilizes the Cu₂O from further photocorrosion. Including isopropanol as a hole scavenger has a drastic effect on the photocorrosion of Cu₂O nanoparticles and suppresses the release of Cu²⁺ ions to the solution. Methodwise, the present data exemplify that EPR and ASV can be useful tools to help quantitatively understand the solid–solution interface photocorrosion phenomena for Cu₂O. Full article

Carbon and metal-oxide nanoparticles (NP) are currently synthesized worldwide for various applications in the solar-energy, optical, pharmaceutical, and biomedical industries, among many others. Gas phase methods comprise flame synthesis and flame spray pyrolysis (FSP), which provide high efficiency, low cost, and the possibility of large-scale applications. The variation of combustion operation parameters exerts significant effects on the properties of the NPs. An analysis of the latest research results relevant to NP flame synthesis can provide new insight into the optimization of these methods and the development of these techniques for a large scale. This review offers insight into the current status of flame synthesis for carbon and metal-oxide NPs—specifically containing analysis and comparison of the most common carbon and metal-oxide NP production techniques. The burner configurations used at the laboratory scale and large scale are also discussed, followed by the assessment of the influence of combustion parameters on the properties of NPs. Finally, the features of the measurement techniques applied for determining NP properties were described. Full article

ABO₃ perovskites offer versatile photoactive nano-templates that can be optimized towards specific technologies, either by means of doping or via heterojunction engineering. SrTiO₃ is a well-studied perovskite photocatalyst, with a highly reducing conduction-band edge. Herein we present a Double-Nozzle Flame Spray Pyrolysis (DN-FSP) technology for the synthesis of high crystallinity SrTiO₃ nanoparticles with controlled La-doping in tandem with SrTiO₃/CuO-heterojunction formation. So-produced La:SrTiO₃/CuO nanocatalysts were optimized for photocatalysis of H₂O/CH₃OH mixtures by varying the La-doping level in the range from 0.25 to 0.9%. We find that, in absence of CuO, the 0.9La:SrTiO₃ material achieved maximal efficient photocatalytic H₂ production, i.e., 12 mmol g⁻¹ h⁻¹. Introduction of CuO on La:SrTiO₃ enhanced selective production of methane CH₄. The optimized 0.25La:SrTiO₃/0.5%CuO catalyst achieved photocatalytic CH₄ production of 1.5 mmol g⁻¹ h⁻¹. Based on XRD, XRF, XPS, BET, and UV-Vis/DRS data, we discuss the photophysical basis of these trends and attribute them to the effect of La atoms in the SrTiO₃ lattice regarding the H₂-production, plus the effect of interfacial CuO on the promotion of CH₄ production. Technology-wise this work is among the first to exemplify the potential of DN-FSP for scalable production of complex nanomaterials such as La:SrTiO₃/CuO with a diligent control of doping and heterojunction in a single-step synthesis. Full article

A flame spray pyrolysis (FSP) technique was applied to obtain pure and Nb(V)-doped nanocrystalline β-Ga₂O₃, which were further studied as gas sensor materials. The obtained samples were characterized with XRD, XPS, TEM, Raman spectroscopy and BET method. Formation of GaNbO₄ phase is observed at high annealing temperatures. Transition of Ga(III) into Ga(I) state during Nb(V) doping prevents donor charge carriers generation and hinders considerable improvement of electrical and gas sensor properties of β-Ga₂O₃. Superior gas sensor performance of obtained ultrafine materials at lower operating temperatures compared to previously reported thin film Ga₂O₃ materials is shown. Full article

In the current research, the productivity of CO₂ photoreduction has been boosted by performing the reaction in an innovative photocatalytic reactor, which allows for operation up to 20 bar. A set of photocatalysts were used, including three types of pristine TiO₂, i.e., one commercially prepared (Evonik P25), one home-prepared by flame spray pyrolysis (FSP), and one obtained by the hydrolysis of TiCl₄ (TiO₂exCl), a bare thermo-exfoliated carbon nitride (C₃N₄-TE), and binary materials composed of TiO₂ and C₃N₄-TE. The photoreduction was carried out in water at pH 14 and in the presence of Na₂SO₃ as a hole scavenger. Hydrogen and very small amounts of CO were detected in the head space of the photoreactor, while in the liquid phase, the main product was formic acid, along with traces of methanol and formaldehyde. The composites P25/TE and TiO₂exCl/TE were found to have a higher productivity if compared to its single constituents used alone, probably due to the heterojunction formed by coupling the two materials. Moreover, the high pressure applied in the photoreactor proved to be very effective in boosting the yield of the organic products. Full article

Flame spray pyrolysis (FSP) is a promising approach to generate nanoparticles from precursor solutions, where the convective droplet heating and evaporation of the single precursor solution droplet play a key role. Depending on the precursor solution under consideration, reactions inside the liquid may occur. The present numerical study concerns the heating, evaporation, and thermal decomposition of single droplets of iron(III) nitrate nonahydrate (INN) and ethanol at an initial temperature of 293.15 K in hot convective air at atmospheric pressure. If the ambience is below the thermal decomposition temperature ($T_{\mathrm{th}}$) of the INN, iron nitrate particles are directly formed inside the particle, whereas at ambient temperatures beyond $T_{\mathrm{th}}$, the iron nitrate thermally decomposes into gaseous Fe₂O₃ and N₂O₅. Vaporization and thermal decomposition govern the process, depending on the droplet surface temperature. If the ambient temperature is larger than a specific value $T^{+}$, thermal decomposition is very fast and vaporization dominates the total process time, whereas at lower ambient temperatures, the vaporization is slower, which causes a lower final droplet surface temperature, leading to considerably longer thermal decomposition, which dominates the total process time under that condition. The ambient temperature at which this reversed behavior occurs depends on initial INN loading of the particle and the relative velocity but is largely independent of the initial droplet size. These new results are very useful in choosing the process temperature, which is recommended to lie beyond the ambient air temperature of $T^{+}$ to assure that the total process time is kept short. The numerical results are parameterized for use in more complex simulations of FSP. Full article

The complete conversion of NO_x to harmless N₂ without N₂O formation is crucial for the control of air pollution, especially at low temperatures. Cu-based catalysts are promising materials due to their low cost and high activity in NO dissociation, even comparable to noble metals; however, they suffer from low stability. Here, we established a Cu-Ce catalyst in one step with strong metal–support interaction by the flame spray pyrolysis (FSP) method. Almost 100% NO conversion was achieved at 100 °C, and they completely transferred into N₂ at a low temperature (200 °C) for the FSP-CuCe catalyst, exhibiting excellent performance in NO reduction by CO reaction. Moreover, the catalytic performance can stay stable, while 23% NO conversion was lost in the same condition for the one made by the co-precipitation (CP) method. This can be attributed to the synergistic effect of abundant active interfacial sites and more flexible surface oxygen created during the FSP process. The flame technology developed here provides an efficient way to fabricate strong metal–support interactions, exhibiting notable potential in the design of stable Cu-based catalysts. Full article

In this work, we take on an in-depth characterization of the complex particle structures made by spray flame synthesis. Because of the resulting hierarchical aggregates, very few measurement techniques are available to analyze their primary particle and fractal properties. Therefore, we use small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM) to investigate the influence of the precursor concentration on the fractal structures of zirconia nanoparticles. The combination of information gained from these measurement results leads to a detailed description of the particle system, including the polydispersity and size distribution of the primary particles. Based on our findings, unstable process conditions could be identified at low precursor concentrations resulting in the broadest size distribution of primary particles with rough surfaces. Higher precursor concentrations lead to reproducible primary particle sizes almost independent of the initial precursor concentration. Regarding the fractal properties, the typical shape of aggregates for aerosols is present for the investigated range of precursor concentrations. In conclusion, the consistent results for SAXS and TEM show a conclusive characterization of a complex particle system, allowing for the identification of the underlying particle formation mechanism. Full article