Formation Of Surface Structures Research Articles

Structural Changes in High-Entropy Alloys CoCrFeNi and CoCrFeMnNi, Irradiated by He Ions at a Temperature of 700 °C.

High-entropy alloys (HEA) are promising structural materials that will successfully resist high-temperature irradiation with helium ions and radiation-induced swelling in new generations of nuclear reactors. In this paper, changes in the elemental and phase composition, surface morphology, and structure of CoCrFeNi and CoCrFeMnNi HEAs irradiated with He2+ ions at a temperature of 700 °C were studied. Structural studies were mainly conducted using the X-ray diffraction method. The formation of a porous surface structure with many microchannels (open blisters) was observed. The average diameter of the blisters in CoCrFeMnNi is around 1.3 times smaller than in CoCrFeNi. It was shown that HEAs' elemental and phase compositions are stable under high-temperature irradiation. It was revealed that, in the region of the peak of implanted helium, high-temperature irradiation leads to the growth of tensile macrostresses in CoCrFeNi by 3.6 times and the formation of compressive macrostresses (-143 MPa) in CoCrFeMnNi; microstresses in the HEAs increase by 2.4 times; and the dislocation density value increases by 4.3 and 7.5 times for CoCrFeNi and CoCrFeMnNi, respectively. The formation of compressive macrostresses and a higher value of dislocation density indicate that the CoCrFeMnNi HEA tends to have greater radiation resistance compared to CoCrFeNi.

Ageing of commercial austenitic, martensitic and duplex stainless steel surfaces after formation of laser-induced periodic surface structures by fs-laser irradiation

The time-dependent wetting behavior was investigated for commercially available austenitic, martensitic and duplex stainless steel surfaces after femtosecond (fs) laser irradiation. For this purpose, highly regular LIPSS with almost identical geometric properties were generated on the stainless steels in an air environment by near-infrared fs-laser processing (λ = 1025 nm, τ = 300 fs, frep = 100 kHz, v = 0.67 m/s, Δx = 6 μm, F=1.1 J/cm2) and compared to the polished initial surfaces as reference. The wetting with distilled water was evaluated as a function of aging time by contact angle measurements using the sessile drop method. The laser-induced morphological, topographical and chemical alteration of the surface was characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, glow-discharge optical emission spectroscopy as well as high-resolution imaging and scanning transmission electron microscopy. Despite an almost identical LIPSS-based topography alteration, the stainless steels revealed very different ageing behavior. For permanently used samples, it was shown that the ageing effect is less pronounced than for samples that were stored in ambient air following fs-laser irradiation until the wetting measurement. The results obtained make an important contribution to understanding and controlling the ageing effect of metal surfaces and thus facilitate the transfer of LIPSS-based functional surface engineering and design to industrial processes.

Study on bulge structure formation mechanisms of laser remelting in air atmosphere

As a key feature of a part or assembly, surface structure can effectively improve the surface properties of the workpiece. Laser remelting is a promising method for surface structure formation, but sensitive to ambient gases. Therefore, this paper presents a numerical model that incorporates the contribution of air atmosphere on surface bulge structure formation. For this, the model couples a concentration field to reflect the oxygen mass transfer in the melt pool and introduces a semi-empirical function to describe the contribution of oxygen to the surface tension. Based on the model, it discusses the surface structure formation mechanisms, the heat-mass transfer characteristics, the melt flow patterns, and the surface force transient evolutions. The results reveal that the action of air atmosphere on melt flow manifests itself through two mechanisms, namely, the enhancement of inward thermocapillary forces and the introduction of outward solutocapillary forces. Furthermore, combined with the laser remelting experiments on 304 stainless steels, the established model is validated concerning the surface bulge structure size, the melt pool depth, and the oxygen distribution.

Reversible Laser Imprinting of Phase Change Photonic Structures in Integrated Waveguides.

Formation of laser-induced periodic surface structures (LIPSS) is known as a fast and robust method of functionalization of material surfaces. Of particular interest are LIPSS that manifest as periodic modulation of phase state of the material, as it implies reversibility of phase modification that constitute rewritable LIPSS, and recently was demonstrated for chalcogenide phase change materials (PCMs). Due to remarkable properties of chalcogenide PCMs─nonvolatality, prominent optical contrast and ns switching speed─such novel phase change LIPSS hold potential for exciting applications in all-optical tunable photonics. In this work we explore phase change LIPSS formation in thin films of Ge2Sb2Te5 (GST) integrated with planar and rib waveguides. We demonstrate that by fine-tuning laser radiation, the morphology of phase change LIPSS can be controlled, including their period and fill factor, and investigate the limitations of multicycle rewriting of the structures. We also demonstrate the formation of phase change LIPSS on a 1D waveguide, which has potential for use as tunable Bragg filters or structures for on-demand light decoupling into the far-field. The presented concept of applying phase change LIPSS offers a promising approach to enable fast and simple tuning in integrated photonic devices.

Simulation of femtosecond laser-induced periodic surface structures on fused silica by considering intrapulse and interpulse feedback

The formation of laser-induced periodic surface structures (LIPSSs) on fused silica upon irradiation with plane wave, double pulse, spot processing, and scanning processing (pulse duration tp = 35 fs, center wavelength λ = 800 nm, low repetition rate ≈1 kHz) is studied theoretically with an improved three-dimensional finite-difference time-domain plasma model. The model covers both intrapulse feedback under single shot and interpulse feedback under multi-shots, thus enabling better prediction of transient responses during laser–material interaction and the evolution of the ablated morphology and accumulated defects’ density with more shots. In simulations of a single plane wave, a double pulse can modulate LIPSS periodicity. In simulations of spot processing with Gaussian beam, an increase in the number of shots results in a noticeable ablation pattern where high-spatial-frequency LIPSS surrounds low-spatial-frequency LIPSS at a fluence of 2.8 J/cm2. Moreover, simulations of scanning processing with Gaussian beam showcase the broad applicability of this model, revealing that the orientation of the LIPSS depends on the polarization direction rather than the scanning path. This new model provides a powerful tool to simulate the formation of LIPSS on silica, particularly when temporally modulated laser is involved or predicting the evolution of morphology dependent on the number of shots.

SUPERHYDROPHOBIC AND ANTIBACTERIAL COATINGS ON VARIOUS COTTON FABRICS USING ZNO AND AESO

Superhydrophobic coatings on cotton utilized in medical applications like hospital gowns and bed linens to offer a protective barrier against fluids and bacteria. Masks were worn with different types of materials. In this study, various cotton employed ZnO and AESO to effectively decrease the surface energy of cotton fabric via a Schiff base reaction. This chemical transformation resulted in the formation of a textured surface structure that exhibited robust adhesion qualities. The study demonstrates that the superhydrophobic coating on silk fabric increases 153. 59%. The coating on silk provides a reference for fabric types with ZnO and AESO coatings.

Efficient Ablation, further GHz Burst Polishing, and Surface Texturing by Ultrafast Laser

A large variety of ultrafast laser‐matter interaction regimes and different processed surface finishing qualities of stainless steel can be achieved by varying the laser processing parameters. The optimization of the laser fluence to the most efficient ablation also leads to the lowest surface roughness of the ablated material. High laser fluence together with a high pulse repetition rate leads to heat accumulation, which results in the formation of microstructures with various morphology and scales. The use of GHz bursts allows a rough stainless‐steel surface to be smoothed and even polished. In this work, the fast and high‐quality milling of 2.5D cavities is demonstrated. Laser beam spot optimization is used to increase the throughput of the high‐power femtosecond laser (67.8 W), resulting in an ablation rate of 13 mm3 min−1. The complex cavities are produced by laser milling and cutting in layers. The formation of surface structures on stainless steel because of laser irradiation has been demonstrated. The possibilities of further GHz burst polishing are examined on previously laser‐milled stainless steel using with lowest possible surface roughness. The ability to polish the surface with microstructures below the original roughness is demonstrated by bursts of ultrashort pulses with a repetition rate in the GHz range. It has been demonstrated that mold milling in stainless steel designed for LED diffusers can be fabricated using a modern femtosecond laser source together with beam size optimization technique for efficient ablation with low surface roughness, layer‐by‐layer milling techniques, and GHz burst polishing techniques.

Polarization and kinetics of optical emission during laser induced periodic surface structure formation on crystalline silicon

Polarization and kinetics of secondary optical emission, which occurs during the formation of laser-induced periodic surface structures (LIPSSs) on crystalline silicon by a femtosecond laser beam in air, were analyzed. It was found that the emission lines of ablated Si atoms and formed in plasma SiN molecules are unpolarized, and they decay on the nanosecond scale. The second harmonic generation (SHG) is enhanced by laser-induced surface plasmons, and the SHG polarization basically repeats the polarization of the laser. The results can be used for optical monitoring of LIPSS formation in real time, which is especially important for laser processing of large non-planar surfaces.

Electrochemical and semiconducting properties of multifunctional smart conductive fabrics based on polypyrrole

AbstractWe have fabricated multifunctional conductive fabrics composed of polypyrrole/BaTiO3/poly(acrylonitrile‐co‐methylacrylate) (PPy/BaTiO3/P(AN‐co‐MA)(PBA) utilizing a simple process including dip coating and in situ chemical polymerization of pyrrole, which oxidized both ammonium persulfate (APS) and ammonium persulfate + iron (III) chloride (APS + FeCl3) for flexible and wearable textile applications. The influence of the oxidant nature, PPy content, and BaTiO3 on the surface structures, electrochemical, and semiconducting characteristics of the fabrics was examined using scanning electrochemical microscopy (SEM), electrochemical impedance spectroscopy (EIS), and the Mott–Schottky (M–S) studies. The study revealed that the size of the polymer nanostructures on fabric has an impact on the electrochemical impedance properties. Specifically, a decrease in diameter (when FeCl3 + APS is used) or the formation of more compact swelling surface structures (when only APS is used) is associated with changes in the conductivity of the coated fabric. Based on the EIS tests, the composite coating (S0.1, S0.2, and S0.3) with FeCl3 has a higher electrical conductivity compared to the coating with APS (PBA). The M–S tests indicate that the semiconducting characteristics of coated fabrics are dependent upon the kind of oxidant, the amount of PPy, and the presence of BaTiO3.

Investigating the transition from high to low spatial frequency periodic nanoripples on TiO2 (0 0 1) oriented surface upon irradiation with UV-femtosecond pulses

The formation of laser-induced periodic surface structures (LIPSS) on a TiO2 (001) oriented surface upon irradiation with UV-fs laser pulses was analyzed. Two systems of low spatial frequency LIPSS (LSFL) perpendicular to the direction of laser polarization are observed after N = 5 laser pulses. One was developed on the edges of the crater created by the first laser pulse, while the other appeared in the center of crater and spread towards the edges. When N was greater than 10, the two LIPSS systems merge. Both LSFL systems have a spatial period of approximately 200 nm and are due to the coherent superposition of surface waves scattered on inhomogeneities of a transient metallic surface. However they differ by the type of defects involved in the excitation process of surface waves. While a pronounced and localized rim triggered LSFL on the edge of the laser spot, LSFL in the central part nucleated at the shallow high spatial frequency LIPSS (HSFL), which are parallel to the laser polarization. A mechanism is proposed to explain the role of the HSFL in the formation of LSFL. Numerical simulations of the absorbed laser power density support the evolution from HSFL to LSFL as the number of laser pulses increased.

Impact of helium and hydrogen plasma exposure on surface damage and erosion of tungsten

The impact of helium plasma exposure on the tungsten surface damage structure development and erosion has been investigated by comparing the impact of hydrogen plasma exposure. Crystal orientation dependence of the undulating surface structure formation and erosion rate is observed on the plasma-exposed tungsten surface independently from the plasma species. The top surface of the plasma exposed tungsten has a tendency to {100} plane independently from the initial surface orientation. Although hydrogen and/or helium cause no erosion in tungsten under incident ion energy exposure conditions below the sputtering threshold, inevitable minute impurities, like oxygen, play an essential role in erosion, and significant erosion can be observed even at 30 eV.

Cost-effective superhydrophobic ZnO films with adjustable wetting behaviors deposited via solution precursor plasma spray process

In this work, ZnO films featuring hierarchical micron−/nanometer-sized structures were deposited for adjusting wettability by a simple solution precursor plasma spray (SPPS) process using cost-effective zinc acetate solution. The effects of solution flow rate on the surface microstructures, surface roughness, crystalline orientation, and wetting behaviors of the films were investigated comprehensively. The results showed that high solution flow rate facilitated the formation of apparent hierarchical surface structures featuring more uniformly-distributed micron-sized protrusions and higher surface roughness. The increase of solution flow rate also promoted the crystalline growth along the non-polar (100) plane. With the solution flow rate increasing from 10 ml/min to 40 ml/min, the synergy of the surface structures and crystalline growth orientation resulted in a sharp decrease of the surface energy of the films from ~74.4 mJ/m2 to ~12.6 mJ/m2 and a dramatic elevation of water contact angles from ~130° to ~155°. The wetting states of different films were elucidated by correlating the wetting behaviors with the surface structures. The SPPS-deposited ZnO films showed high adhesion to water droplets, similar to the wetting behaviors of the petal effect, which could be used as a “mechanical hand” for non-loss microdroplet transfer. The work shows that SPPS represents a promising method to deposit cost-effective superhydrophobic films with adjustable wetting behaviors.

Surface blackening of titanium alloy by laser nanosecond pulses

The possibility of developing and blackening the surface of titanium alloy by nanosecond pulses of an ArF laser, a Nd:YAG laser, and a copper vapor laser for use in space engineering is studied in this work. For various irradiation regimes, the optimal parameters for the formation of the necessary surface structures were determined. The possibility of applying a reliable color layer without the use of any paints on the surface of a titanium alloy as a result of treatment with an Nd:YAG laser beam is shown. In particular, this method of laser processing will make it possible to obtain black color on the surface of devices used in outer space to absorb and dissipate solar energy, and it is expected to increase the radiation resistance of such coatings and their service life.

Oxidation-driven 2D LIPSS on amorphous Si films atop metal layers: The interplay of near-field and far-field effects

We investigate the formation of Laser-Induced Periodic Surface Structures (LIPSS) on amorphous Si films coated on Al using circularly polarized femtosecond lasers. By controlling laser fluence, we induce oxidation-based surface patterns, with their regularity governed by the interplay between near-field and far-field contributions. Achieving the right balance between these effects results in a consistent hexagonal pattern. Varying the underlying metal type further revealed its impact on pattern quality: strong far-field contributions led to irregular patterns, while dominant near-field effects resulted in extensive oxidation. Our study reveals the critical balance between near-field and far-field effects in optimizing 2D LIPSS patterns, emphasizing the role of the underlying metal.

The effect of molten pool evolution on the formation of surface structures during laser polishing

As a novel surface treatment technology, in-situ laser polishing aims to improve surface finish of 3D printed parts, while laying the foundation for the integrated processing of 3D printing and laser polishing. However, the polishing process will introduce a few new surface structures (undercuts, step structures, ripples, etc.), which will affect the surface roughness. In this work, the surface roughness and surface structure after high power and low power polishing were compared respectively through experiments. In addition, a 2D transient numerical model was developed to explore the forming mechanism of different structures. The evolution of temperature field, velocity field and freedom surface of melting pool under different parameters were analyzed by the model. The results showed that the solidification induced surface structure with large roughness was generated after high power polishing. During its formation, the thermocapillary force was dominant and drove the tangential flow of fluid. While, low power polishing resulted in ripple structure with small roughness. The emergence of this structure was primarily due to the capillary force as the leading force in the melting pool flow process, which drove the normal flow of the melt, thus eliminating the large surface curvature. Furthermore, the width of the melting pool in the simulation was compared with the width of the single scanning track, and they were in good agreement. Finally, by adjusting the test strategy, it was found that the surface roughness could reach the lowest (0.88 ± 0.06 μm) only when the two structures coexisted.

Porosity Engineering of Dried Smart Poly(N-isopropylacrylamide) Hydrogels for Gas Sensing.

A recent study unveiled the potential of acrylamide-based stimulus-responsive hydrogels for volatile organic compound detection in gaseous environments. However, for gas sensing, a large surface area, that is, a highly porous material, offering many adsorption sites is crucial. The large humidity variation in the gaseous environment constitutes a significant challenge for preserving an initially porous structure, as the pores tend to be unstable and irreversibly collapse. Therefore, the present investigation focuses on enhancing the porosity of smart PNiPAAm hydrogels under the conditions of a gaseous environment and the preservation of the structural integrity for long-term use. We have studied the influence of polyethylene glycol (PEG) as a porogen and the application of different drying methods and posttreatment. The investigations lead to the conclusion that only the combination of PEG addition, freeze-drying, and subsequent conditioning in high relative humidity enables a long-term stable formation of a porous surface and inner structure of the material. The significantly enhanced swelling response in a gaseous environment and in the test gas acetone is confirmed by gravimetric experiments of bulk samples and continuous measurements of thin films on piezoresistive pressure sensor chips. These measurements are furthermore complemented by an in-depth analysis of the morphology and microstructure. While the study was conducted for PNiPAAm, the insights and developed processes are general in nature and can be applied for porosity engineering of other smart hydrogel materials for VOC detection in gaseous environments.

Chemical and Topographical Changes upon Sub‐100‐nm Laser‐Induced Periodic Surface Structure Formation on Titanium Alloy: The Influence of Laser Pulse Repetition Rate and Number of Over‐Scans

Titanium and its alloys are known to allow the straightforward laser‐based manufacturing of ordered surface nanostructures, so‐called high spatial frequency laser‐induced periodic surface structures (HSFL). These structures exhibit sub‐100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi‐method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near‐infrared ps‐laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near‐surface chemical analyses hard X‐ray photoelectron spectroscopy (HAXPES) and depth‐profiling time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non‐ablative laser‐induced near‐surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat‐accumulation effects.

Formation of two-dimensional laser-induced periodic surface structures on titanium by GHz burst mode femtosecond laser pulses

GHz burst mode femtosecond (fs) laser pulses, which consist of a series of pulse trains with ultra-fast intervals of several hundred picoseconds, have offered distinct features for material processing compared to conventional irradiation of laser pulses (single-pulse mode). We apply GHz burst mode processing to fabricate laser-induced periodic surface structures (LIPSS) on the material surfaces. In our previous work for silicon (Si), we have found that GHz burst mode can create unique two-dimensional (2D) LIPSS composed of both parallel and perpendicular to the laser polarization direction. We proposed that the formation of 2D-LIPSS is attributed to the synergetic contributions of electromagnetic and hydrodynamic mechanisms. To further investigate more detailed formation mechanisms and explore practical applications, we employ titanium (Ti), whose properties are significantly different from Si. We demonstrate that GHz burst mode fs laser pulses (central wavelength: 1,030 nm, intra-pulse width: 230 fs, intra-pulse repetition rate (an intra-pulse interval): 4.88 GHz (205 ps) and burst pulse repetition rate: 10 kHz) can also fabricate 2D-LIPSS on Ti surfaces. We attribute the dominant formation mechanism of 2D-LIPSS to the generation of hot spots with highly enhanced electric fields due to transient change of material properties during GHz burst pulse irradiation. Based on this speculation, properly tailoring the shapes of the burst pulse with an optimum intra-pulse number enables the creation of well-defined 2D-LIPSS. Furthermore, essentially homogeneous 2D-LIPSS can be formed in a large area by laser scanning of a focused fs laser beam with a stage scanning speed of 5 mm/s.

Numerical study of ultrafast optical instability causing structured light absorption in metal

We present the first-principle numerical study of nonlinear decay of a femtosecond laser pulse into a pair of surface plasmon polaritons (SPP) during reflection from a rough metallic surface. The ultrafast dynamics of the decay was studied at damaging laser fluences of about 1 J/cm2, and the principal role of the electronic collision rate growth was proved. The resulting strongly inhomogeneous heating of metal is an important stage of laser-induced phenomena like ablation, terahertz radiation generation, and periodic surface structures formation.

Tributyrin microcapsule prepared by ultrahigh methoxylated pectin combination with maltodextrin: The characterization, gastrointestinal digestion, and fecal fermentation behavior

A modified ultrahigh methoxylated pectin (UHMP, DM>90%) combined with maltodextrin was used to prepare tributyrin microcapsules. The encapsulation performance of microcapsules and their potential application in gut health were investigated in this study. Results showed that tributyrin was successfully encapsulated into the matrix of microcapsules, and there is no extensive chemical reaction occurred during encapsulation. The UHMP is conducive to the dispersion of tributyrin, while the maltodextrin as wall material promoted the formation of smooth surface structure of microcapsules. Microencapsulation is able to provide thermal protection for tributyrin, as reflected by the increased decomposition temperature and the decreased weight loss rate. In addition, microencapsulation effectively masks the unpleasant odor of tributyrin, resulting in a significantly reduced off-odor retention rate. During small intestinal digestion, the UHMP-stabilized tributyrin emulsions partly demulsified and led to the release of tributyrin, however, a significant higher tributyrin retention rate (88.1 ± 1.3%) was observed in UHMP-stabilized tributyrin emulsions when compared with the blank group (60.1 ± 4.6%). Through in vitro fecal fermentation, it was found that UHMP-stabilized tributyrin emulsions can regulate bacterial community by stimulating the growth of probiotics (e.g. Lachnospira, Phascolarctobacterium, and Parabacteroides) and decreasing the relative abundances of harmful microbes (e.g. Klebsiella and Fusobacterium). Furthermore, UHMP-stabilized tributyrin emulsions promote the production of SCFAs, especially, the content of butyric acid increased from 1.59 ± 0.32 mmol/L to 10.58 ± 1.89 mmol/L. The present study provides a feasible approach for the preparation of tributyrin microcapsule, which improves its application performance in gut health.