Deposition Of Nanoparticles Research Articles

Plasmonic ZnO-Au Nanocomposites: A Synergistic Approach to Enhanced Photocatalytic Activity through Nonthermal Plasma-Assisted Synthesis

A novel and efficient method for synthesizing Au-decorated ZnO nanoparticles (NPs) with enhanced photocatalytic activity is presented. The synthesis involves a two-step process: hydrothermal preparation of ZnO NPs followed by nonthermal plasma-assisted deposition of Au nanoparticles on their surface. Comprehensive characterization of the ZnO and ZnO–Au NPs was carried out using X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Optical properties were evaluated via UV-Vis absorption and fluorescence measurements. The synthesized ZnO NPs displayed a hexagonal wurtzite structure, and the successful deposition of Au NPs was confirmed by TEM and XPS analysis, along with Raman and fluorescence data showing the quenching effect caused by Au. The incorporation of Au nanoparticles led to the appearance of localized surface plasmon resonance (LSPR) at 540 nm, enhancing visible light absorption and improving photocatalytic performance. Notably, the methylene blue (MB) degradation efficiency increased from 78% with pure ZnO NPs to 91.6% with ZnO–Au NPs under UV-Vis irradiation, demonstrating superior photocatalytic activity. This study introduces a simple and scalable method for synthesizing plasmonic ZnO-Au hybrid nanomaterials using plasma technology and highlights the critical role of Au NPs in enhancing photocatalytic performance by reducing electron–hole recombination.

Construction of ternary hierarchical heterostructures with favorable interfacial compatibility for ultrahigh photocatalytic H2O2 production

Sluggish charge transfer dynamics are still the key issue limiting the development of photocatalysis. In this study, CdS/ZnIn2S4/MIL-53-NH2 ternary hierarchical heterostructures were constructed via a building block approach, where ZnIn2S4 lamellae first grow on MIL-53-NH2 followed by CdS nanoparticle deposition. The favorable interfacial compatibility and ternary heterostructures contribute to rapid and multistep spatial charge transfer, which suppresses charge recombination. Therefore, ultrahigh H2O2 production of 1792 μmol·L−1 was obtained over CdS/Znln2S4/MIL-53-NH2 composites with visible light, pure water and ambient air, which is not only higher than that of each monomer and binary heterostructure but also better than those of most reported references. Notably, the apparent quantum yield reached 4.5 % at 400 nm, and the solar-to-H2O2 conversion efficiency was 0.081 % in pure water and ambient air. Additionally, H2O2 generation over CdS/Znln2S4/MIL-53-NH2 composites involves two-electron O2 reduction with ·O2- as an intermediate. This work may encourage heterostructure design for efficient photocatalytic H2O2 production.

Unique flake-shaped sulfur morphology favored by the binder-free electrophoretically deposited TiO2 layer as a promising cathode structure for Li-S batteries

Metal oxides have been extensively studied as catalyst additives in Li-S batteries due to their high affinity for soluble lithium polysulfides (LiPSs). The present study developed a novel carbon nanomaterials- and binder-free 3D sulfur host by electrophoretic deposition (EPD) of TiO2 nanoparticles on carbon fiber paper (CFP). Benefiting from the unique well-connected TiO2 porous layer formed by EPD, the initial discharge capacity of Li-S battery was increased from 1160 mAh g−1 in conventional cast TiO2/binder/S cathode (Cast:CFP/PVDF/TiO2/S) to 1310 mAh g−1 in the EPD:CFP/TiO2/S cathode, along with an overpotential drop of 16 %. Electron microscopic studies at 100% state-of-charge (SoC) revealed that while notorious sulfur particulates were formed on Cast:CFP/PVDF/TiO2/S, the surface of EPD:CFP/TiO2/S was covered with flake-shaped sulfur precipitates. The formation of sulfur flakes effectively suppressed pulverization in EPD:CFP/TiO2/S, leading to superior electrochemical performance and cycle life. Microstructural studies and real-time EIS investigations revealed that sulfur flakes nucleated across the Li2S matrix at the initial stages of charge and grew vertically from the sulfur/TiO2 interface. The preferential growth mechanism of sulfur flakes was attributed to the superior surface conductance of the EPD-TiO2 film enabled by the ordered clusters formed during EPD, enhancing the kinetics of electrocatalytic reactions of polysulfides at the TiO2/sulfur interface. Our results show that developing novel methods to modify the morphology of secondary sulfur upon cycling is critical for enhancing charge-discharge performance in Li-S batteries.

Enhancement of corrosion, biocompatibility and drug delivery properties of nitinol implants surface by Al-Zn-LDH nanohybrids

This study investigates the enhancement of drug delivery and corrosion resistance by incorporating dexamethasone sodium phosphate into aluminum-zinc layered double hydroxide (LDH) coated nickel-titanium alloys. The nickel-titanium samples were fabricated from titanium and nickel powders using spark plasma sintering (SPS) and cold press sintering (CPS), followed by electrophoretic deposition of LDH nanoparticles. This composite construction aims to utilize the biocompatibility and mechanical properties of nickel-titanium, combined with the controlled drug release and corrosion resistance properties of LDH coatings. Structural and microstructural characterizations were performed using X-ray diffraction and scanning electron microscopy. The results indicated that SPS samples exhibited superior microstructural homogeneity and corrosion resistance compared to CPS samples. Dexamethasone sodium phosphate was successfully intercalated into the LDH layers, as evidenced by an increase in layer spacing from 7.14 Å to 20.130 Å. The LDH-coated nickel-titanium with intercalated dexamethasone sodium phosphate demonstrated a 5 % lower drug release rate and significantly improved corrosion resistance compared to uncoated samples. Cell adhesion studies confirmed good biocompatibility between cells and the coated surface. This composite material shows promise for enhanced performance in biomedical applications, particularly in drug delivery and corrosion resistance.

Hierarchically Structured Cellulose Acetate@Silk Protein Membrane with Enhanced Mechanical and Electromagnetic Interference Shielding Performances.

Compared to conventional fibers, electrospun porous nanofibers with hierarchical structures often involve additional active sites, interfaces, and internal spaces which boost the performances of functional materials. Here in this study, coaxial composite cellulose acetate@silk fibroin (CA@SF) fibrous membranes are constructed through an electrostatic spinning technique combining solvent-induced phase separation. Hierarchical core-shell structures on the fibers are achieved, which significantly increases the surface area and benefits the mechanical property, flux, as well as the electroless deposition of Ag nanoparticles. The total electromagnetic shielding efficiency of the sandwiched hierarchical CA@SF@Ag composite membrane with a thickness of only 100 μm reaches up to 100 dB, surpassing around 82% beyond nonhierarchical ones. To be noticed, when post-treated by ethanol, the membrane enables an enhanced tensile strength of up to 10 MPa with a thickness of only 50 μm. Our findings pave the way to the application of electrospun fiber membranes in the field of ultrathin electromagnetic shielding films.

Ternary ZnS/ZnO/Graphitic Carbon Nitride Heterojunction for Photocatalytic Hydrogen Production.

Ternary ZnS/ZnO/graphitic carbon nitride (gCN) photocatalysts were prepared by coupling gCN sheets with ZnO nanorods under solvothermal conditions followed by sulfurization using Na2S. SEM and TEM analyses show that small-sized ZnS particles (ca. 7.2 nm) deposit homogeneously on the surface of ZnO/gCN nanohybrids. Photoluminescence and electrochemical impedance spectroscopy show that ZnS allows for an enhanced charge separation efficiency as well as prolonged lifetime of photogenerated charge carriers, leading to improved hydrogen photoproduction under UV light irradiation compared to ZnO/gCN. Moreover, the deposition of ZnS nanoparticles improves the photostability of the ZnS/ZnO/gCN catalyst for hydrogen production. A double Z-scheme mechanism is proposed for hydrogen photoproduction using the ZnS/ZnO/gCN heterojunction.

Discrete element model of nanoparticle deposition during electrospraying

Electrospraying is a technique for the production and deposition of nanoparticles. However, deposited layer morphology is strongly dependent on the operating conditions and hard to predict. Here, we present a spatially 3D model based on the Discrete Element Method (DEM) with the analytical evaluation of interparticle forces and drag force and the numerical evaluation of electric force. The developed connection between mesh-free DEM and mesh-based Finite Volume Method (FVM) used for the evaluation of electric potential field enables to lower the computational time while maintaining accuracy of the predictions We focus on modelling the influence of interparticle forces on particle deposition and deposited layer morphology, which are phenomena usually neglected in the literature so far. Preferential landing of particles is indicated to be a consequence of both electric force and Van der Waals forces. Contact particle interactions allow particle stacking (creating thus fractal-like structure) or allow falling down of particles and their rearrangement (leading to compact layers).

Silicon Nanowire Biosensors for Diabetes Mellitus Monitoring

The main goal of this research is the development of a label-free biosensor for the detection of diabetes mellitus (DM) using the target molecule retinol-binding protein 4 (RBP4). The enzyme-linked immunosorbent assay (ELISA) approach, currently used to detect DM, is time-consuming and difficult. As a result, label-free biosensors are being considered as an alternative. In this research, silicon nanowires (SiNWs) were selected as the transducer for this biosensor due to their low cost, real-time analysis capability, high sensitivity, and low detection limit. The SiNWs were created using conventional lithography, reactive ion etching (RIE), and physical vapor deposition (PVD), and then dripped with a gold nanoparticle solution to create gold-decorated SiNWs. The surface of the gold-decorated SiNWs was functionalized using 3-aminothiophenol and glutaraldehyde solutions before being immobilized with DM RBP4 antibodies and targets. The electrical characterization of the gold nanoparticle decorated SiNWs biosensor revealed good performance in DM detection. The pH tests confirmed that the SiNWs acted as a transducer, with current proportional to the DM RBP4 concentration. The estimated limit of detection (LOD) and sensitivity for detecting DM RBP4 binding were 0.076 fg/mL and 8.92 nA(g/mL)-1, respectively. This gold nanoparticle decorated SiNWs biosensor performed better than other methods and enabled efficient, accurate, and direct detection of DM. The SiNWs could be used as a distinctive electrical protein biosensor for biological diagnostic purposes. In conclusion, gold nanoparticle deposition offers effective label-free, direct, and high-accuracy DM detection, outperforming previous approaches. Thus, these SiNWs serve as novel electrical protein biosensors for future biological diagnostic applications.

Target-mediated silver deposition-based electrochemical biosensor for highly sensitive detection of human chorionic gonadotropin

As a glycoprotein hormone, human chorionic gonadotropin (hCG) is an established marker for pregnancy test. On the basis of the target-mediated silver deposition (TSD), in this work, we report the development of an amplification-free electrochemical biosensor for the highly sensitive detection of hCG. The detection of hCG involves the use of the affinity peptide-modified electrode for hCG capture (the CGGSSPPLRINRHILTR peptide containing the hCG-binding domain of the PPLRINRHILTR sequence is used as the affinity peptide), the oxidation of the diol sites of the glycan chains on hCG hormones into aldehyde groups by NaIO4, and the deposition of silver nanoparticles (AgNPs) for the solid-state voltammetric stripping analysis. Due to the deposition of multiple AgNPs while the solid-state Ag/AgCl voltammetric process has a high signal-to-noise ratio, the TSD-based electrochemical biosensor can be applied to the highly sensitive detection of hCG without the need for signal amplification. Under optimal conditions, the stripping current increased linearly with an increasing hCG concentration over the range from 1.0 to 25 mIU/mL, with a detection limit of 0.45 mIU/mL. Owing to the high specificity of the hCG-binding peptide PPLRINRHILTR, this electrochemical hCG biosensor exhibits high selectivity. The results of the quantitative assay of hCG in urine samples at the concentrations of 25, 10, and 1.0 mIU/mL are desirable, indicating the good anti-interference capability. As the TSD-based electrochemical biosensor allows the amplification-free detection of low-abundance hCG, it is easy to use and cost-effective, showing great promise in point-of-care assay of hCG for pregnancy test.

Silver nanoparticles bridging liquid metal for wearable electromagnetic interference fabric

Stretchable conductive fibers are essential for the advancement of wearable electronic textiles. However, a significant challenge arises as their conductivity sharply decreases when stretched due to disruptions in electronic transport. Coating fibers with soft liquid metal (LM) has emerged as a promising solution. Despite this, there remains an urgent need to develop methods that enhance LM adhesion to substrates while facilitating efficient electron transport pathways. This study demonstrates a novel Ag-LM conductive network strategy for fabricating a thermoplastic polyurethane/polydopamine/silver-LM (TPU/PDA/Ag-LM) fiber membrane. This membrane exhibits outstanding stretchable electromagnetic interference (EMI) shielding performance and is produced through straightforward electrospinning, electroless depositing, and LM coating and activation. The TPU/PDA/Ag fiber membrane is initially prepared via polydopamine-assisted deposition of silver nanoparticles (AgNPs) on electrospun TPU fibers. The presence of AgNPs on the surface of TPU/PDA fibers enhances LM adhesion to the substrate and bridges adjacent LM to establish efficient conductive paths. This interaction benefits from the reactive alloying between AgNPs and LM, where the LM infiltrates the gaps among AgNPs, forming a distinctive LM-Ag alloy layer that uniformly coats the surface of TPU fibers. As anticipated, the unique three-dimensional (3D) interconnected LM-Ag conductive network remains intact during stretching, ensuring strain-invariant conductivity. The fabricated TPU/PDA/Ag-LM fiber membrane demonstrates exceptional EMI shielding effectiveness (SE) of 77.4 dB within the frequency range of 8.2–12.8 GHz and maintains an excellent EMI SE of 37.2 dB under extensive tensile deformation of 300%. Furthermore, the TPU/PDA/Ag-LM fiber membrane shows remarkable mechanical properties and stable Joule heating performance even under significant stretching.

Superhydrophobic and antibacterial larch wood prepared by PEI controlled growth of conical ZnO nanopillar

The natural antibacterial performance of cicada wings inspired the morphology design and application of zinc oxide (ZnO) nanoparticles on wood surfaces to enhance combined antibacterial function. The commonly interior used larch wood was chosen as base material and firstly pre-treated with ultrasonic-hydrothermal method, the deposition of ZnO nanoparticles with different morphologies was controlled by polyethyleneimine (PEI) concentration during the crystal growth, and the analysis of surface characteristics and antibacterial efficacy was fully tested. Scanning Electron Microscopy (SEM) observations revealed that the addition of PEI altered the morphology of ZnO nanoparticles on the wood surface. ZnO structures without PEI exhibited hexagonal prismatic shapes. As the PEI concentration increased, the particle size of ZnO decreased. When 6 mmol/L of PEI was added, ZnO transformed into a conical structure. Contact angle measurements confirmed the preparation of superhydrophobic ZnO, which exhibited self-cleaning properties. The antibacterial circle method test results showed that superhydrophobic ZnO wood prepared with 6 mmol/L of PEI exhibited superior antibacterial properties, with higher activity against Staphylococcus aureus compared to Escherichia coli. Overall, the study demonstrates a promising approach to developing polyfunctional and effective antibacterial wood surfaces inspired by natural cicada wings nanostructures.

Targeted photothermal cancer therapy using surface-modified transition metal dichalcogenides

Breast cancer, particularly triple-negative breast cancer (TNBC), is the most impactful cancer affecting women, necessitating continuous evaluation of enhanced treatment methods. In this study, we synthesized a folic acid-modified gold nanoparticle-MoSe2 composite (FAM) by liquid exfoliation using glycyrrhizic acid (GA), spontaneous reduction of AuNP, and linkage between folic acid and AuNP using EDC/NHS coupling. With the assistance of GA, MoSe2 nanosheets can be easily exfoliated in aqueous solutions and exhibit biocompatibility. In addition, the gold nanoparticle deposition on the nanosheet was spontaneously induced due to the electron transfer property of MoSe2. Folic acid was used as a targeting molecule because triple-negative breast cancer (TNBC) lacks the common breast cancer markers. We investigated the effectiveness of photothermal therapy using FAM, which enhances light-heat transfer through the synergistic effect of gold and GA-exfoliated MoSe2 (GM). The nanomaterials exhibited improved photothermal conversion efficiency of 62.2 %, high thermal stability, and increased cellular uptake ratio. Subsequently, when the FAM reached the tumor microenvironment, the materials successfully entered the cells through folate receptor-mediated endocytosis and generated heat to kill cells under an 808 nm laser (0.8 W cm−2) by apoptosis. The biocompatibility and photothermic activity of FAM were determined in vitro by a tetrazolium salt assay, live/dead cell staining, cellular uptake ratio, and flow cytometry with human TNBC cells (MDA-MB-231). In summary, the FAM showed a more advanced therapeutic effect than GM in all outcomes. Our findings indicate that FAM has the potential to be used as a biomaterial for anticancer therapy.

Enhancing Pregnancy Care: Harnessing Label‐Free Immunosensors for Pre‐Eclampsia Detection Using PdNPs/Poly(3,5‐Diaminobenzoic Acid) Modified Glassy Carbon Electrodes

AbstractPlacental Growth factor (PlGF) is one of the biomarkers useful for detecting pregnancy hypertension disorder, Pre‐eclampsia. Herein, we focus on developing a label‐free immunosensor using simple electrochemical methods to detect PlGF antigens for pre‐eclampsia diagnosis. The work includes the electrochemical deposition of Palladium nanoparticles (PdNPs) on the glassy carbon electrode (GCE) surface using amperometry followed by electropolymerization of diaminobenzoic acid (DABA) onto the PdNPs/GCE. Antibody (aPlGF) was covalently immobilized on the pDABA/PdNPs/GCE using EDC/NHS reaction. The interaction of the antibody with the antigen was measured using differential pulse voltammetric technique. The linear range obtained for the immunosensor is 1–25 ng mL−1 with a limit of detection of 53 pg mL−1. The stability and reproducibility of the sensor were obtained in the acceptable range. The developed sensor was used to detect PlGF antigen in artificial blood and urine samples by spike recovery analysis.

Fabrication and in vitro biocompatibility of hierarchical cellulose acetate/polyvinylpyrrolidone@titania nanowire hollow microfibers

In this study, hierarchical cellulose acetate/polyvinylpyrrolidone hollow microfibers (CA/PVP HMFs) were first prepared via a dip coating method using a steel wire as tubular template and then supported a sol-gel deposition of titania nanoparticles (NPs) to derive CA/PVP@titania NP HMFs. After hydrothermally treated in NaOH solution, CA/PVP@titania NP HMFs were transformed to CA/PVP@titania nanowire (NW) HMFs. SEM observation showed that CA/PVP@titania NW HMFs had a hollow structure with diameters of 450–600 μm and exhibited a hierarchical and nanofibrous structure. Their surfaces were constructed by numerous titania NWs with diameters of 10–30 nm and lengths of 1–5 μm. The incorporation of PVP not only caused a significant change in surface wettability from hydrophobic CA HMFs to hydrophilic CA/PVP HMFs, but also promoted the sol-gel deposition of titania NPs on CA/PVP HMFs. CA/PVP@titania NW HMFs exhibited the highest hydrophilicity with water contact angle of 32° and the largest specific surface area of 86.1 m2/g. In vitro biocompatible evaluation indicated that CA/PVP@titania NW HMFs exhibited much higher cell adhesion and proliferation than CA/PVP@titania NP HMFs and CA/PVP HMFs within 7 days due to the presence of nanofibrous surface architecture. Thus, the present CA/PVP titania NW HMFs have potential as biocompatible cell supporting matrices.

Study on the inhibitory behavior of high-voltage electric field on the agglomeration and sedimentation of nanoparticles in suspension

Nanoparticles can improve the heat transfer effect of fluids, however, they are difficult to dissolve in the base fluid and are prone to fouling, agglomeration and sedimentation during flow, which affects their efficient heat transfer characteristics. In this paper, the inhibitory effect of high-voltage electric field on the agglomeration and deposition of TiO2 nanoparticles in suspension was comparatively studied by comprehensive gravity sedimentation, spectrophotometer, particle size analysis, and zeta potential method. Studies have shown that the absorbance of suspensions is basically the same in neutral and acidic environments. However, in a highly alkaline environment, the agglomeration rate of nanoparticles increases significantly, resulting in a decrease in the absorbance of the suspension. The high-voltage non-uniform electric field generated by the active Cu rod electrode can effectively inhibit the agglomeration of TiO2 nanoparticles. However, the suppression effect of an external electric field is not necessarily the higher the voltage, the better. Different nanomaterials have different critical voltages. The high-voltage electric field of 1 kV has the best inhibitory effect on the agglomeration and deposition of TiO2 nanoparticles. An in-depth analysis of the mechanisms of the movement and agglomeration of TiO2 particles in suspension under high-voltage electric field excitation was conducted. The result shows that the agglomeration and sedimentation of particles in suspension depend on the Zeta potential of the nano particles. The higher the absolute value, the more stable the dispersion system is.

Silicon surface texturing via TBAB-SDS composite additives enhanced copper-assisted chemical etching

Uneven etching and low fabrication efficiency impede the large-scale applications of copper-assisted chemical etching (Cu-ACE) for texturing light-trapping structures on the surface of silicon wafers. To address this, a composite additive composed of tetrabutylammonium bromide (TBAB) and sodium dodecyl sulfate (SDS) was introduced into the Cu-ACE system. The results indicated that TBAB accelerated the etching rate and improved the texturing uniformity, while SDS enlarged the size of the formed structures and enhanced their ultraviolet light absorption efficiency. The prepared inverted pyramid structure reduced the reflectivity of the silicon wafer surface to 3.8 %, thus exhibiting efficient light-trapping capabilities. The etching evolution under various TBAB concentrations and different HF/H2O2 ratios was studied by characterizing the surface contact angle and copper deposition morphology. The results indicated that electrostatic attraction between TBAB and dangling bonds on the silicon wafer surface enhanced material transfer at the reaction interface and changed the electron distribution around dangling bonds, thus facilitating the catalytic metal attack on these bonds. The copper ion reactivity was decreased due to complexation between the dissociated alkyl sulfate ions of SDS and copper ions, which favored the deposition of larger copper nanoparticles during etching, thereby increasing the size of structures. This research offers valuable insights to enable the large-scale applications of Cu-ACE.

Tribological behavior and lubrication mechanism of polyalphaolefin with added Cu-Ni bimetallic nanoparticles on a TiN coating

In this study, the tribological behavior of TiN coatings lubricated with a polyalphaolefin (PAO)-based oil containing Cu-Ni bimetallic nanoparticles was investigated under a maximum contact pressure of 0.9 GPa in reciprocating ball-on-disk mode. The addition of 0.1 wt% Cu-Ni nanoparticles to PAO6 reduced the friction coefficient to 0.018 and also decreased the wear rate of TiN coatings to 4.23 × 10-7 mm3/Nm. X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy revealed the deposition of Cu-Ni nanoparticles and carbon-based tribofilms on the contact region of the tribopairs. These originated from the tribo-induced degradation of the polyalphaolefin molecule in PAO6 + 0.1 %Cu-Ni nanoparticles, which helped decrease the COF and wear. Moreover, a comparative analysis suggested that the presence of nickel in the Cu-Ni nanoparticles had a catalytic effect during sliding. They facilitated the in situ formation of carbon-based film due to the degradation of polyalphaolefins under the combined effects of frictional heat and contact stress, demonstrating a self-repair capability.

Integrating Cu2O Colloidal Mie Resonators in Structurally Colored Butterfly Wings for Bio-Nanohybrid Photonic Applications.

Colloidal Cu2O nanoparticles can exhibit both photocatalytic activity under visible light illumination and resonant Mie scattering, but, for their practical application, they have to be immobilized on a substrate. Butterfly wings, with complex hierarchical photonic nanoarchitectures, constitute a promising substrate for the immobilization of nanoparticles and for the tuning of their optical properties. The native wax layer covering the wing scales of Polyommatus icarus butterflies was removed by simple ethanol pretreatment prior to the deposition of Cu2O nanoparticles, which allowed reproducible deposition on the dorsal blue wing scale nanoarchitectures via drop casting. The samples were investigated by optical and electron microscopy, attenuated total reflectance infrared spectroscopy, UV-visible spectrophotometry, microspectrophotometry, and hyperspectral spectrophotometry. It was found that the Cu2O nanoparticles integrated well into the photonic nanoarchitecture of the P. icarus wing scales, they exhibited Mie resonance on the glass slides, and the spectral signature of this resonance was absent on Si(100). A novel bio-nanohybrid photonic nanoarchitecture was produced in which the spectral properties of the butterfly wings were tuned by the Cu2O nanoparticles and their backscattering due to the Mie resonance was suppressed despite the low refractive index of the chitinous substrate.

Esterification-Induced Spontaneous Deposition of Nanoparticle Monolayers on Substrates with Percolation Network Morphology.

Nanoparticle monolayers (NPMLs) exhibit unique collective properties that are highly desirable for applications in sensors, catalysts, and optics. However, their practical use is often hindered by structural instability, especially when they are exposed to solvents. In this study, we developed a method for the spontaneous deposition of gold nanoparticle monolayers (AuNPMLs) on silicon substrates via covalent bonding interactions that provides excellent structural stability in solvents with varying polarities. The esterification reaction between carboxyl-functionalized gold nanoparticles and alkyl-chloride-functionalized silicon substrates spontaneously forms AuNPMLs on the substrate in which single-crystalline domains are interconnected, forming a percolation network morphology. The ex situ scanning electron microscopy measurements show that the surface coverage of AuNPMLs rapidly increases up to ca. 60% during the initial 10 min, followed by gradual growth and saturation at ca. 70% at 360 min of deposition time. On the other hand, the single-crystalline domain size reaches its maximum at 45 min and then gradually decreases, which may be attributed to the desorption of AuNPs by the hydrolysis of ester bonds. The reflectance spectra of AuNPMLs showed the red shift as the deposition time increases up to 45 min with a subsequent blue shift thereafter, which is consistent with the change of the single-crystalline domain size with the deposition time. The covalent bonding interaction-mediated nanoparticle deposition method can be used to form stable AuNPMLs with controlled surface coverage and domain size, allowing for fine control of the optical properties and possibly other properties. The excellent structural stability of AuNPMLs and their controlled properties may provide new opportunities for practical applications of NPMLs.

A new method for estimating nanoparticle deposition coverage from a set of weak-contrast SEM images

Imaging nanomaterials in hybrid systems is critical to understanding the structure and functionality of these systems. However, current technologies such as scanning electron microscopy (SEM) may obtain high resolution/contrast images at the cost of damaging or contaminating the sample. For example, to prevent the charging of organic substrate/matrix, a very thin layer of metal is coated on the surface, which will permanently contaminate the sample and eliminate the possibility of reusing it for following processes. Conversely, examining the sample without any modifications, in pursuit of high-fidelity digital images of its unperturbed state, can come at the cost of low-quality images that are challenging to process. Here, a solution is proposed for the case where no brightness threshold is available to reliably judge whether a region is covered with nanomaterials. The method examines local brightness variability to detect nanomaterial deposits. Very good agreement with manually obtained values of the coverage is observed, and a strong case is made for the method's automatability. Although the developed methodology is showcased in the context of SEM images of Polydimethylsiloxane (PDMS) substrates on which silicone dioxide (SiO2) nanoparticles are assembled, the underlying concepts may be extended to situations where straightforward brightness thresholding is not viable.