Control Of Surface Morphology Research Articles

Antifouling Properties of Electrospun Polymeric Coatings Induced by Controlled Surface Morphology

Nosocomial infections affect implanted medical devices and greatly challenge their functional outcomes, becoming sometimes life threatening for the patients. Therefore, aggressive antibiotic therapies are administered, which often require the use of last‐resort drugs, if the infection is caused by multi‐drug‐resistant bacteria. Reducing the risk of bacterial contamination of medical devices in the hospitals has thus become an emerging issue. Promising routes to control these infections are based on materials provided with intrinsic bactericidal properties (i.e., chemical action) and on the design of surface coatings able to limit bacteria adhesion and fouling phenomena (i.e., physical action), thus preventing bacterial biofilm formation. Here, we report the development and validation of coatings made of layer‐by‐layer deposition of electrospun poly(vinylidene fluoride‐co‐trifluoro ethylene) P(VDF‐TrFE) fibers with controlled orientations, which ultimately gave rise to antifouling surfaces. The obtained 10‐layer surface morphology with 90° orientation fibers was able to efficiently prevent the adhesion of bacteria, by establishing a superhydrophobic‐like behavior compatible with the Cassie‐Baxter regimen. Moreover, the results highlighted that surface wettability and bacteria adhesion could be controlled using fibers with diameter comparable to bacteria size (i.e., achievable via electrospinning process), by tuning the intra‐fiber spacing, with relevant implications in the future design of biomedical surface coatings.

Effects of experimental in-office bleaching gels incorporated with co-doped titanium dioxide nanoparticles on dental enamel physical properties.

To evaluate the physical properties of enamel submitted to hydrogen peroxide (HP) incorporated with titanium dioxide nanoparticles (NP) co-doped with nitrogen and fluorine and irradiated with violet LED light (LT). Enamel-dentin disks were randomly allocated (T0) into groups, according to HP (HP6, HP15, or HP35) and NP (no NP, 5NP, or 10NP) concentrations, and irradiated or not with LT. A negative control (NC) group was set. After three bleaching sessions (T1, T2, and T3), specimens were stored in saliva for 14days (T4). Enamel surface microhardness number (KHN), surface roughness (Ra), cross-sectional microhardness (ΔS), energy-dispersive spectroscopy (EDS), scanning electron (SEM), and polarized light (PLM) microscopies were performed. Surface KHN was significantly influenced by NP over time, independently of LT irradiation. At T3 and T4, gels with 5NP and 10NP exhibited no KHN differences compared to NC and baseline values, which were not observed under the absence of NP. NP incorporation did not statistically interfere with the ΔS and Ra. PLM images exhibited surface/subsurface darkening areas suggestive of demineralizing regions. SEM demonstrated some intraprismatic affection in the groups without NP. EDS reported a higher enamel calcium to phosphorus ratio following 10NP gels applications. Gels with NP maintained the enamel surface microhardness levels and seemed to control surface morphology, upholding the mineral content. None of the proposed experimental protocols have negatively influenced the enamel surface roughness and the cross-sectional microhardness.

Controlled Wrinkle Patterning on Thin Films to Improve Hydrophobicity.

Controlling surface morphology is one of the main strategies used to tune surface hydrophobic and icephobic properties. Taking advantage of coating growth by initiated chemical vapor deposition, random and ordered wrinkles were induced on a thin film of polyperfluorodecyl acrylate (pPFDA) deposited on polydimethylsiloxane (PDMS) to simultaneously modify surface chemistry and morphology. A range of wrinkles of different wavelengths were studied, and how the wrinkle characteristics change with varying coating thickness. Ordered wrinkles enhanced hydrophobicity more when compared to random wrinkles, with a noticeable effect for coating thickness on the order of hundreds of nanometers. An insight into the mechanism of surface wrinkling and its effect on freezing delay is also provided, and promising results were found on ordered wrinkles, where a freezing delay was observed.

High-speed electrolyte jet 3D printing of ultrasmooth and robust Cu microelectrodes

Electrochemical 3D printing technology built on computer numerical control platforms has enabled multi-dimensional and multi-scale manufacturing of various metal materials through layered electrochemical deposition. Compared to thermal 3D printing technology, electrolyte meniscus-confined 3D printing can manufacture Cu microstructures with fewer defects and smoother surfaces. In the meantime, it is still susceptible to unstable liquid–solid-air interfaces, low deposition rates, and limited printing geometry. This work combined jet electrochemical deposition with a portable 3-axis platform to develop a cyclic high-speed electrolyte jet (HSEJ) 3D printer. It offers a faster deposition rate of 53.4 µm/h when printing ultrasmooth Cu microelectrodes with surface average roughness down to 1.1 nm and microhardness of 3.3 GPa which is much higher than the best result of 2.4 GPa obtained by the other ECD methods. It is identified that the fluctuation of cathode current density plays a crucial role in defining the nucleation morphology on the Cu surface, while the cathode current efficiency is a reliable indicator to assess the deposition localization by reflecting the variation of diffusion percentage. HSEJ 3D printing provides a sustainable pathway for the facile recycling of waste cables into high-grade metal microelectronics with controllable surface morphology and 3D dimensions.Graphical

Controlling surface morphology of Ag-doped ZnO as a buffer layer by dispersion engineering in planar perovskite solar cells

In recent years, the power conversion efficiency (PCE (%)) of perovskite solar cells (PSCs) has improved to over 26%. To enhance the photovoltaic properties of PSCs, several materials for the electron transport layer (ETL) have been investigated. Zinc oxide (ZnO) is a significant ETL due to its high electron mobility and optical transparency in PSCs. As a result of various deposition methods, ZnO ETL can be processed at low temperatures. On the other hand, based on several studies, metal-doped ZnO can facilitate electron transfer, thereby improving the performance of un-doped ZnO ETL-based PSCs. Here, to improve the PCE (%) and long-term stability of un-doped ZnO ETL-PSCs, silver (Ag)-doped ZnO 1wt% as a buffer layer is examined. In this paper, with the addition of an organic solvent (ethanol) to the dispersion of Ag-doped ZnO 1 wt% nanoparticles (NPs) in deionized (DI) water, the morphology of the buffer layer (Ag-doped ZnO 1 wt%) can be controlled. This approach focuses on reducing the wettability of the ZnO/Ag-doped ZnO 1 wt% bilayer ETLs and enhancing the stability of un-doped ZnO ETL-PSCs. According to the results, the ZnO/H2O-ethanol mixtures-Ag-doped ZnO 1 wt% bilayer ETL leads to the formation of high-quality perovskite with low defects, reducing the recombination rate, and long-term stability of un-doped ZnO ETL-PSCs in ambient conditions.

Plasma-Chemical Method of Silicon Carbide Modification to Obtain Particles with Controlled Surface Morphology

Plasma-Chemical Method of Silicon Carbide Modification to Obtain Particles with Controlled Surface Morphology

Off the Grid: A new strategy for material-jet 3D printing with enhanced sub-droplet resolution

Drop-on-Demand additive manufacturing could offer a facile solution for scalable on-site manufacturing. With an increasing number of functional materials available for this technology, there are growing opportunities for applications, such as electronics. Here we report on a novel printing strategy, Off-the-Grid (OtG), which enables refined positioning of individual droplets and enhanced resolution compared to the traditional printing strategy. We demonstrate successful printing of structures with feature position control smaller than a single droplet size, and hence enhanced shape fidelity for intricate designs. This strategy is extended to filled patterns, enabling improved layer coverage and customisable inter-layer droplet positioning to control surface morphology. The OtG strategy is applied to produce functional designs, such as conformable circuitry and miniaturized antennae, and is transferable to different materials, from metal nanoparticle and polymeric inks on inkjet platforms, to molten metals on a MetalJet printer. These results could advance exploitation of AM in electronics, wearable electronics, medical devices, and metamaterials.

Preparation of Polyurethane–Urea Fibers with Controlled Surface Morphology via Gel State

It is widely known that skin irritation can be induced by interactions between polymer fibers constituting clothing and the skin, leading to skin inflammation and unfavorable dermatological reactions. Thus, significant endeavors have been directed toward ameliorating this phenomenon. This study engineered synthetic fibers with reduced potential for skin irritation. This was achieved via a strategy inspired by the inherent smoothness of silk fibers, which exhibit minimal friction and irritation against the skin. This investigation focused on urethane fibers, a class of synthetic fibers frequently used in textile applications. Hydrogel cross-linked polyurethane–urea fibers were subjected to controlled swelling in different hydrophilic mixed-solvent environments. Subsequent freeze-drying procedures were employed to yield fibers with diverse surface morphologies and encompassing features such as elevations and creases. The correlation between the compositions of the solvent mixtures used and the resulting surface morphologies of the fibers was rigorously assessed through polarized light and scanning electron microscopies. Additionally, the interplay between the degree of swelling and the tensile strength of the fabricated fibers was comprehensively analyzed. Consequently, the methodological combination of swelling and freeze-drying endowed the polyurethane–urea fibers with various surface profiles. Future studies will delve into the intricate connection between fiber surface characteristics and their potential to induce skin irritation. It is envisaged that such investigations will substantially contribute to the refinement of textile fibers designed for enhanced compatibility with the skin.

Controlling Superhydrophobicity on Complex Substrates Based on a Vapor-Phase Sublimation and Deposition Polymerization.

The superhydrophobic properties of material surfaces have attracted significant research and practical development in a wide range of applications. In the present study, a superhydrophobic coating was fabricated using a vapor-phase sublimation and deposition process. This process offers several advantages, including a controllable and tunable superhydrophobic property, a dry and solvent-free process that uses well-defined water/ice templates during fabrication, and a coating technology that is applicable to various substrates, regardless of their dimensions or complex geometric configurations. The fabrication process exploits time-dependent condensation to produce ice templates with a controlled surface morphology and roughness. The templates are sacrificed via vapor sublimation, which results in mass transfer of water vapor out of the system. A second vapor source of a polymer precursor is then introduced to the system, and deposition occurs upon polymerization on the iced templates, replicating the same topologies from the iced templates. The continuation of the co-current sublimation and deposition processes finally renders permanent hierarchical structures of the polymer coatings that combine the native hydrophobic property of the polymer and the structured property by the sacrificed ice templates, achieving a level of superhydrophobicity that is tunable from 90° to 164°. The experiments demonstrated the use of [2,2]paracyclophanes as the starting materials for forming the superhydrophobic coatings of poly(p-xylylenes) on substrate surfaces. In comparison to conventional vapor deposition of poly(p-xylylenes), which resulted in dense thin-film coatings with only a moderate water contact angle of approximately 90°, the reported superhydrophobic coatings and fabrication process can achieve a high water contact angle of 164°. Demonstrations furthermore revealed that the proposed coatings are durable while maintaining superhydrophobicity on various substrates, including an intraocular lens and a cardiovascular stent, even against harsh treatment conditions and varied solution compositions used on the substrates.

Defect-Rich SnO2 Nanofiber as an Oxygen-Defect-Driven Photoenergy Shield against UV Light Cell Damage.

Usually, most studies focus on toxic gas and photosensors by using electrospinning and metal oxide polycrystalline SnO2 nanofibers (PNFs), while fewer studies discuss cell-material interactions and photoelectric effect. In this work, the controllable surface morphology and oxygen defect (VO) structure properties were provided to show the opportunity of metal oxide PNFs to convert photoenergy into bio-energy for bio-material applications. Using the photobiomodulation effect of defect-rich polycrystalline SnO2 nanofibers (PNFs) is the main idea to modulate the cell-material interactions, such as adhesion, growth direction, and reactive oxygen species (ROS) density. The VO structures, including out-of-plane oxygen defects (op-VO), bridge oxygen defects (b-VO), and in-plane oxygen defects (ip-VO), were studied using synchrotron analysis to investigate the electron transfer between the VO structures and conduction bands. These intragrain VO structures can be treated as generation-recombination centers, which can convert various photoenergies (365-520 nm) into different current levels that form distinct surface potential levels; this is referred to as the photoelectric effect. PNF conductivity was enhanced 53.6-fold by enlarging the grain size (410 nm2) by increasing the annealing temperature, which can improve the photoelectric effect. In vitro removal of reactive oxygen species (ROS) can be achieved by using the photoelectric effect of PNFs. Also, the viability and shape of human bone marrow mesenchymal stem cells (hMSCs-BM) were also influenced significantly by the photobiomodulation effect. The cell damage and survival rate can be prevented and enhanced by using PNFs; metal oxide nanofibers are no longer only environmental sensors but can also be a bio-material to convert the photoenergy into bio-energy for biomedical science applications.

Bacterial cellulose-based film with self-floating hierarchical porous structure for efficient solar-driven interfacial evaporation

Interface solar water evaporation is a mean of rapidly evaporating water using solar energy. However, it is still a challenge to obtain solar evaporators with simple assembly, durability and high photothermal performance. Here, we demonstrated an effective post foaming strategy for treating nitrogen-doped reduced graphene oxide/bacterial cellulose film (F-NRGO@BC) prepared by a simple in situ culture method. The composite film contains hierarchical porous structure and bubbles on the film, achieving an integrated self-floating interface evaporator with excellent light absorption (96.5 %) and high toughness (200.18 kJ m−3). Porous structure and low enthalpy of F-NRGO@BC make a high evaporation rate of 1.68 kg m−2 h−1 and a low thermal conductivity of 0.644 W m−1 K−1 to ensure effective energy efficiency and heat insulation. This design of controlling surface morphology and internal structure provides a novel way for large-scale preparation and high-performance evaporator.

Utilizing Hydrazine and Hydrogen as Reducing Agents to Control the Nanoscale Surface Morphology of the Palladium Thin Films

A key challenge facing fabrication of nanomaterials is the ability to precisely control the surface morphology of the nanostructures through exploitation of process parameters. In this study, palladium thin films with carefully controlled surface morphologies are obtained through the careful choice of the reducing agent used during the pre‐plating activation step in the three‐step autocatalytic electroless plating consisting of 1) surface functionalization; 2) surface activation; and 3) deposition of the film onto alumina substrates. It is important to note that the reducing agents that influenced the surface morphology of the palladium thin films are employed in the pre‐plating activation step instead of the widely utilized electroless deposition step. It is revealed in the high‐resolution scanning electron microscope results that the hydrogen reducing agent yields a dense film with 3D spheroidal morphologies with an average cluster size of ≈415 nm while the hydrazine reducing agent produces a very smooth uniform surface morphology consisting of extremely small grains. The obtained results can be exploited in controlling and tailoring the surface‐dependent properties of the palladium thin film for applications in gas sensors, detectors, or palladium‐based membranes.

Fast One-Step Fabrication of Highly Regular Microscrolls with Controllable Surface Morphology.

Although rolling origami technology has provided convenient access to three-dimensional (3D) microstructure systems, the high yield and scalable construction of complex rolling structures with well-defined geometry without impeding functionality has remained challenging. The straightforward, one-step fabrication that uses external mechanical stress to scroll micrometer thick, flexible planar films with centimeter lateral dimensions into tubular or spiral geometry within a few seconds is demonstrated. The method allows controlling the scrolls' diameter, number of windings and nanostructured surface morphology, and is applicable to a wide range of functional materials. The obtained 3D structures are highly promising for various applications including sensors, actuators, microrobotics, as well as energy storage and electronic devices.

2D Ti3C2 MXene interfaced ZnO/WO3 thin film nanostructures towards improved photoelectrochemical water splitting

We explored the morphology evolution approach for sustained photoelectrochemical (PEC) water splitting by developing dual heterojunction. Herein, novel ZnO/WO3/Ti3C2 photoelectrode has been developed for the first time by the integration of flake-like ZnO, nanocrystal featured WO3, and layer-structured two-dimensional (2D) Ti3C2 MXene morphologies towards PEC activity under simulated solar light. By adjusting the radio frequency (RF) magnetron sputtering and post-annealing, flake-like/nanocrystals featured ZnO/WO3 heterostructure observed with uniform growth of WO3 nanocrystals over the flake-like ZnO. Further, efficient integration of layer-structured 2D Ti3C2 MXene on ZnO/WO3 was provided through spin-coating. Utilizing robust surface interface between ZnO, WO3, and Ti3C2, optical transmittance and band gap have been modified. Accordingly, ZnO/WO3/Ti3C2 improved the photocurrent generation about 1.4 × 10−3 A/cm2 compared to pure ZnO (7.8 × 10−4 A/cm2) and ZnO/WO3 (1.1 × 10−3 A/cm2) at +0.4 V. These findings further provided a photoconversion efficiency of 1.16 % by the ZnO/WO3/Ti3C2 at +0.4 V. The PEC studies proved that electrically conductive Ti3C2 MXene can significantly separate the charge carriers from ZnO/WO3. On the other hand, this morphology-induced architecture proved sustainable surface interaction with KOH electrolyte than Na2SO3 and Na2SO4 media. Overall, the above developments suggest a robust interface in ZnO/WO3/Ti3C2 under controlled surface morphology and PEC water splitting activity.

Integrating Fly Ash-Controlled Surface Morphology and Candle Grease Coating: Access to Highly Hydrophobic Poly (L-lactic Acid) Composite for Anti-Icing Application

New ways of recycling fly ash are of great significance for reducing the environmental pollution. In this work, biodegradable hydrophobic poly (L-lactic acid)/fly ash composites for anti-icing application were successfully fabricated via a facile solvent-volatilization-induced phase separation approach. A silane coupling agent of 3-(Trimethoxysilyl) propyl methacrylate was used to decorate a fly ash surface (FA@KH570) for strengthening the interface bonding between fly ash and poly (L-lactic acid). Moreover, FA@KH570 could obviously enhance the crystallinity of poly (L-lactic acid) (PLLA)/FA@KH570 composites, which accelerated the conversion from the liquid-liquid to the liquid-solid phase separation principle. Correspondingly, the controllable surface morphology from smooth to petal-like microspheres was attained simply by adjusting the FA@KH570 content. After coating nontoxic candle grease, the apparent contact angle of 5 wt% PLLA/FA@KH570 composite was significantly increased to an astonishing 151.2°, which endowed the composite with excellent anti-icing property. This strategy paves the way for recycling waste fly ash and manufacturing hydrophobic poly (L-lactic acid) composite for potential application as an anti-icing material for refrigerator interior walls.

Conductive carbon-polymer composite for bioelectrodes and electricity generation in a sedimentary microbial fuel cell

Biofilm formation on conductive materials for bioelectrodes and electricity production in a microbial fuel cell (MFC) is important for different areas as bioremediation, production of biohydrogen, electricity, energy storage and even biomedical area. The development of conductive composites from residual materials with controlled surface morphology for bioelectroactive bacteria biofilm formation can overcome challenges as biocompatibility, stability, chemical/environmental inertness and low power density in a MFC. In this study a carbon-polymer composite was developed from residual banana peel and a bioelectrode was with electroactive bacteria was successfully obtained and applied as a new conductive material in a sediment microbial fuel cell (SMFC). Cyclic Voltammetry of the bioelectrodes demonstrated the conductive property of the composite and the presence of bioelectroactive biofilm attached. The process to obtain the activated carbon from banana peel was related with the bioelectrodes performances in the SMFC. The composite obtained at 700 °C showed the best results of power density, total chemical oxygen demand removed (TCOD) and coulombic efficiency (CE) of 1056.6 W/m3, 98% TCOD and 23.7% respectively. This power density was 10 times higher than that with a bioanode made with commercial carbon cloth. The feasibility of the electroactive biofilm formation on a carbon-polymer composite was confirmed and the use of banana peel residual for electricity production in a SMFC was proved for the first time.

Cavitation state recognition for control valve using AlexNet-type neural networks with three-channel images transformed by time series

The control valve is a crucial component with high switching frequency in coal liquefaction systems. Its performance exerts a great influence on the long-term operations in the coal chemical technology. Cavitation is a key factor affecting the control accuracy and surface morphology of the control valve; hence, it will further shorten the service life of the control valve. A cavitation state recognition model based on vibration acceleration time series is proposed in this paper, and the cavitation stage in the valve is identified accurately. Three vibration acceleration sensors are attached to the valve seat to measure cavitation-induced vibration data. The collected time series is divided into fragments based on the non-overlap moving window method, and these fragments are converted into feature maps using the Gramian angular field transform. These feature maps are then input into AlexNet to train the cavitation state recognition model. The experimental results show that recognition accuracy could be improved effectively upon the increase in the length of the time series fragment, and the proposed model has a similar prediction accuracy on unfamiliar datasets. Compared with no noise, the recognition accuracy could reach to 95% when the moving window length is 150 and the signal-to-noise ratio is equal to 5 dB. Furthermore, the proposed model could still achieve good recognition results under mixed open conditions.

Controlled Surface Morphology and Electrical Properties of Sputtered Titanium Nitride Thin Film for Metal–Insulator–Metal Structures

Titanium nitride (TiN) is a material of interest for electrodes owing to its high-temperature stability, robustness, low-cost, and suitable electrical properties. Herein, we studied the surface morphology and electrical properties of TiN thin film deposited onto an Si/SiO2 <100> substrate through direct current (DC) sputtering with a high-purity TiN target in an argon-gas environment. The electrical properties and surface morphology of TiN thin film significantly improved with increased source power and decreased working pressure. The improved electrical properties could be attributed to the suppressed secondary phase (Ti2N) formation and the reduced electron scattering on smoother surface. Consequently, high-quality TiN thin film with the lowest resistivity (ρ = 0.1 mΩ·cm) and the smallest surface roughness (RMS roughness, Rq = 0.3 nm) was obtained under the optimized condition. The TiN film was further used as the bottom electrode for a metal–insulator–metal (MIM) capacitor. Results demonstrated that the electrical properties of TiN film were comparable to those of noble-metal thin films. Therefore, the TiN thin film fabricated by DC sputtering method had excellent electrical properties and good Rq, indicating its potential applications in MIM capacitors and Si technology.

Microdroplet-based synthesis of polymethylsilsesquioxane microspheres with controllable size, surface morphology, and internal structure

Monodispersed polysilsesquioxane (PSQ) microspheres are generally synthesized by the classical sol–gel method. Using this method, the particle size is limited to the range of several hundred nanometers to several microns. The preparation of monodispersed large-sized PSQ microspheres remains technically challenging. Herein, with the polymethylsilsesquioxane (PMSQ) microspheres as the model product, a microdroplet-based strategy was developed for the synthesis of PSQ microspheres with larger particle sizes. According to the properties of the reactants, a W/O microdroplet reaction system was realized, i.e., with the mixture of methyltrimethoxysilane (MTMS) and liquid paraffin as the continuous phase and ammonia solution as the dispersed phase. The monodispersed W/O microdroplets were generated in a step T-junction microfluidic device, and solidified into PMSQ microspheres via in-situ interfacial polycondensation (∼2 min) in a microtube reactor. The size, surface morphology and internal structure of the PMSQ microspheres could be tuned by adjusting the synthesis conditions, mainly including the two-phase flow rates, MTMS concentration, NH4OH concentration, and the structural parameters of the microfluidic device. Various PMSQ microspheres with corrugated or smooth surface morphology, and loose or dense internal structure could be synthesized. The microsphere size could be tuned from tens of microns (∼20 μm) to hundreds of microns.

Electrochemical Study of the Electrodeposition of a Dense Nanocrystalline Fe Film from Fe(II) Ions Dissolved in an Ionic Liquid

The electrodeposition behavior of Fe was studied in phenyltrimethylammonium chloride-ethylene glycol eutectic-based ionic liquids (TMPAC-EG EILs) containing FeCl2 through electrochemical measurement and the deposit characterization. Some kinetic parameters (standard rate constants, transfer coefficients and activation energy for standard rate constants) as well as transport properties were obtained and discussed as function of temperature. The values of transfer coefficient (0.32–0.39) are significantly lower than conventional value (0.5). Electrodeposition of Fe follows three-dimensional progressive nucleation and growth mode, which is unaffected by temperature. Besides, it is found that deposition temperature plays a central role in controlling surface morphology and structure of the resultant Fe coatings. At low temperature (333–353 K), smooth and dense iron coating can be obtained. The phase structure changes from a nanocrystalline α-Fe to amorphous phase (metallic glass) as the deposition temperature increases from 333 K to 353 K.