Oxygen Plasma Research Articles

Comparison of the effect of oxygen and nitrogen plasma treatments on the surface activation of PLA/rGO composites

Cold plasma is known as a method to enhance the adsorption of proteins on the surface of biomaterials. In this experimental study, the efficacy of oxygen and nitrogen plasma treatment on the activation of Poly l-lactic acid/reduced graphene oxide composite (PLAG) was investigated. For this purpose, the chemical, physicochemical, and morphological characteristics, ability to adsorb amino acid l-tyrosine, and biological behavior of the oxygen and nitrogen plasma-treated composites (PLAG-O and PLAG-N) were studied. Following the exposure to oxygen and nitrogen plasma, (PLAG-O) composites presented more enhancement in Raman CC and CH bonds. The evaluation of l-tyrosine adsorption revealed the higher intensity of FTIR CN, CC and NH and Raman CH chemical bonds and also lower intensity of l-tyrosine UV absorbance in solution medium for l-tyrosine-adsorbed oxygen plasma-treated (PLAG-Ot) compared to l-tyrosine-adsorbed nitrogen plasma-treated (PLAG-Nt) composites. More apparent l-tyrosine island-shaped zones were appeared all over the surface of PLAG-Ot composites through FE-SEM experiment. Moreover, conducting detailed AFM study revealed a higher difference in surface roughness (Ra) of the PLAG-O and PLAG-Ot (140 nm) compared to the PLAG-N and PLAG-Nt composites (25 nm). From the biological point of view, the oxygen plasma-treated composites presented better HDF cell behavior in terms of viability and attachment, as well. According to the results of this study, the oxygen plasma treatment exhibits a higher potential to activate Poly l-lactic acid–reduced graphene oxide composite surface compared to the surface treatment in nitrogen plasma.

Simple and Rapid Monolayer Self-Assembly of Nanoparticles at the Air/Water Interface.

Colloidal crystals and their two-dimensional (2D) monolayers, which have been commonly applied in nanosphere lithography, have the potential to revolutionize many engineering disciplines; however, current production techniques are hampered by a restricted preparation area, laborious procedures, and the need for advanced equipment. We propose a self-assembly-driven, simple, and low-cost method to prepare 2D colloidal nanosphere monolayers with excellent repeatability across wide regions. The self-assembly capability of colloidal polystyrene (PS) nanospheres at the air/water interface was utilized to transfer the assembled monolayers onto a substrate. This innovative method combines the advantages of methods that permit deposition at the air/water interface, such as Langmuir and drop coating, in order to deliver defect-free, simple-to-install, and simple-to-apply deposition across vast regions. Using field emission scanning electron microscopy and atomic force microscopy, the resultant coatings were characterized. The size of the nanospheres was reduced using an oxygen plasma etch process in an inductively coupled plasma reactive ion etching system, and the reflectance properties of the substrates for various nanosphere sizes were investigated. By evaporation of a thin gold capping layer on the templates, their optical properties were compared using surface-enhanced Raman scattering spectroscopy. This work has the potential to expand the use of nanosphere lithography by offering a simple and reproducible method that eliminates the need for complicated experimental setups and reduces the amount of material required for monolayer coating, thus lowering the cost.

Antiviral and antibacterial efficacy of nanocomposite amorphous carbon films with copper nanoparticles

Copper compound-rich films and coatings are effective against widespread viruses and bacteria. Even though the killing mechanisms are still debated, it is agreed that the metal ion, nanoparticle release, and surface effects are of paramount importance to the antiviral and antibacterial efficacy of the surfaces. In this work we have investigated the behavior of the reactive magnetron sputtered nanocomposite diamond-like carbon thin films with copper nanoparticles (DLC:Cu). The films were etched employing oxygen plasma and/or exposed to ultra-pure water, aiming to investigate the differences of the Cu release in the medium and changes in film morphology. The presence of metallic copper and Cu2O phases was confirmed by multiple analytical methods. Pristine films were more effective in the Cu release reaching up to 1.3 mg/L/cm2 concentration. Plasma processing resulted in the oxidation of the films which released less Cu, but after exposure to water, their average roughness increased more, up to 5.5 nm. Pristine and O2 plasma processed DLC:Cu films were effective against both model coronavirus and herpesvirus after 1-hour contact time and reached virus reductions of up to 2.23 and 1.63 log10, respectively. Pristine DLC:Cu films were more effective than plasma-processed ones against herpesvirus, while less expressed difference was found for coronavirus. The virucidal efficacy over up to 24 h exposures in the aqueous medium was validated. A bactericidal study confirmed that pristine DLC:Cu films were effective against gram-negative E. coli and gram-positive E. faecalis bacteria. After 3 h, 100 % antibacterial efficiency (ABE) was obtained for E. coli and 99.97 % for E. faecalis. After 8 h and longer exposures, 100 % ABE was reached. The half-life inactivation of viruses was 8.10–11.08 min and for E. faecalis 15.1–72.2 min.

An experimental and computational investigation of discharge mode transitions in a partially magnetized radio frequency capacitively coupled oxygen discharge

AbstractA magnetized capacitively coupled oxygen plasma was studied synergistically using phase resolved optical emission spectroscopy and particle‐based kinetic simulation. Discharge mode transitions from ambipolar mode into drift mode and finally into α mode induced by increasing the magnetic field were observed at different driving frequencies and different electrode gaps. The simulation results demonstrate that the discharge operating in the same mode exhibits a similar degree of electronegativity. By increasing driving frequency or electrode gap, the same discharge mode transition tends to occur at a lower magnetic field, and, meanwhile, the high electric field and electron power absorption shift from the bulk region to the sheath edge.

Plasma treated‐double layer electrospun fiber mats from thermoplastic polyurethane and gelatin for wound healing applications

AbstractConventional wound treatment options provide a barrier against exogenous microbial penetration but cannot simultaneously provide an antibacterial characteristic and promote healing. However, bioactive dressings can accelerate wound healing and have an antibacterial effect in addition to being able to cover and protect lesions. In this study, double‐layer thermoplastic polyurethane (TPU)‐gelatin fibrous dressings that mimic the epidermis and dermis layers of the skin were fabricated via electrospinning technique. As a bioactive agent, Hypericum perforatum oil (HPO) was utilized to impart antibacterial and therapeutic properties to the dressings. Tannic acid was also used in fiber mat formulations as a cross‐linking agent. Oxygen plasma treatment was applied as a surface activation technique to improve adhesion of TPU and gelation layers. The fiber structure of the mats was revealed by a scanning electron microscopy (SEM) study. Fourier transform infrared (FTIR) spectroscopy was used to demonstrate HPO loading onto the mats. The water vapor transmission rate (WVTR) and fluid absorbency of the mats were compared with some commercial dressings. According to these results, it can be suggested that the mats can be used for moderate to high exudative wounds. All dressings, even the control sample showed antibacterial features against both Staphylococcus aureus and Escherichia coli bacteria due to the tannic acid. In vitro wound healing assays were carried out on the plasma‐treated sample and it was observed that the sample did not negatively affect the migration and proliferation abilities of the cells which are necessary for wound healing. Overall results indicated that the plasma‐treated fibrous mat would be a good candidate as a wound dressing material having an antibacterial character.

Piezoelectric energy harvesting from the atomic oxygen hypervelocity impact in low Earth orbit

Atomic oxygen (AO) in low Earth orbit (LEO) can cause severe progressive damage to spacecraft orbiting at hypervelocities over 7 km/s; therefore, all space-graded materials need to be qualified for protection against these high energy impacts. Instead of treating AO as a threat, can we use these atomic impacts, which have enough energy to cause material failure, to generate power? Despite its potential, no attempt has yet been made to utilize the hypervelocity impact energy of AO. Thus, we propose a piezoelectric energy harvesting method through the hypervelocity AO impact in LEO. In this study, energy harvesting with various configurations was experimentally demonstrated using a conventional lead zirconate titanate (PZT) ceramic plate under oxygen plasma exposure to simulate AO impact. The average output power density was 4 W/m2 under 1.43 × 1016 atoms/cm2s effective AO flux conditions. Our study provides a new method for generating energy in a space environment with limited energy sources.

Sputter deposition of hydrogen-doped ZnO layers under humid oxygen plasma

Sputter deposition of hydrogen-doped ZnO layers under humid oxygen plasma

Enhancing optical biosensing: Comparing two physical treatments for GPTES chemical functionalization of Cyclo-Olefin Copolymer foil

Cyclo-olefin-copolymer (COC) transparent films are currently the best choice for micro-fluidic bio-sensors for point-of-care diagnostic applications using optical signal detection. However, while the optical and mechanical properties of this polymer are extremely good, the adhesion of the bio-probes on this surface is not optimal, due to its chemical structure, that presents only saturated carbon bonds. The deposition of organo-silane molecules on the COC surface is one of the most effective ways to overcome this problem. But, for the surface functionalization, a surface physical treatment is necessary before the chemical modification of the COC surface. In this paper a comparison of the effectiveness of two different physical treatments, oxygen plasma and UV-ozone, is reported. In particular, the exposure time of the UV-Ozone treatment has been selected to avoid the problem of auto-fluorescence of the modified COC surface, that was observed also for relatively short UV exposure (around 10 min). An investigation of the reactive radicals created on the surface after the physical treatments and the following chemical modification with the organo-silane molecule (GPTES) has been performed using X-ray photoemission spectroscopy. The surface energy and morphology of the films have been also measured by contact angle and optical profilometry. Finally, the bio-probes adhesion performances of the COC surfaces obtained with the two physical treatments and the chemical modification were tested in a fluorescence-based assay, using an organic light emission diode to excite the fluorescence. We observed that the UV-ozone treatment allows to obtain a siloxane network with some reactive epoxy radicals on the COC surface, however, their quantity and distribution are less important and homogeneous than in the oxygen plasma treated surfaces.

Selective removal of single-layer graphene over double-layer graphene on SiO2 by remote oxygen plasma irradiation

Graphene sheet transferred onto the SiO2 substrate has various types at different regions such as single-layer graphene (SLG), double-layer graphene (DLG), and multi-layer graphene (MLG). These layers were identified by Raman analysis of 2D band position around 2700 cm−1 and full width at half maximum (FWHM). The transferred graphene sheets on SiO2 were remotely irradiated by oxygen plasma without energetic ions at a room temperature. At the beginning of the oxygen plasma irradiation, the carbons on the surface of the graphene sheets were oxidized and the 2D-FWHMs were broadened due to an increase of defects on the basal plane. By controlling the plasma irradiation time up to 120 min, selectively stripping away the SLG regions on the SiO2 surface was observed while leaving the other DLG and MLG regions. The difference in attractive forces resulted in favorable desorption of carbon atoms occurred in the oxidized SLG regions on SiO2 surface by the remote oxygen plasma irradiation.

Enhancing bioactivity and biocompatibility of polyetheretherketone (PEEK) for dental and maxillofacial implants: A novel sequential soaking process

Polyetheretherketone (PEEK) exhibits excellent biocompatibility, fatigue resistance, and an elastic modulus similar to bone, presenting broad application prospects in the field of dental and maxillofacial implants. However, the bioinertness of PEEK limits its applications. In this study, we developed a method to generate biocompatible and bioactive PEEK through a simple sequential soaking process, aimed at inducing bone differentiation and enhancing antibacterial properties. Initially, a three-dimensional (3D) porous network was introduced on the PEEK surface by soaking in concentrated sulfuric acid and water. Subsequently, the sulfonated PEEK surface was treated with oxygen plasma, followed by immersion in a dopamine solution to coat a polydopamine (PDA) layer. Finally, polydopamine phosphate ester-modified 3D porous PEEK was obtained through the reaction of phosphoryl chloride with surface phenolic hydroxyl groups. Systematic studies were conducted using scanning electron microscopy, X-ray photoelectron spectroscopy, water contact angle analysis, cell proliferation and adhesion, osteogenic gene expression detection, alkaline phosphatase staining, alizarin red staining, and bacterial culture. Overall, compared to unmodified PEEK, the modified PEEK significantly enhanced in vitro cell proliferation and adhesion, osteogenic differentiation, and antibacterial properties. The simple surface modification measures combined in this study may represent a promising technology and could facilitate the application of PEEK in dental and maxillofacial implants.

The impact of atmospheric air plasma treatment on the polyfunctional end-use polyester fabric using new synthetic pyrazole dye

Before gluing, bonding, and painting, a variety of materials' surfaces can be modified using the widely used plasma treatment technique. These materials include plastics, glass, metals, and wood. Materials' physical and chemical properties are changed in an environmentally responsible way to enhance or confer particular qualities. The recently used technology known as low-temperature atmospheric pressure plasma (LTAPP) allows heat-sensitive materials to be surface modified in a simple, one-step process. Polymer-based materials are frequently surface modified using LTAPP treatment to improve adhesion, printability, and surface sterility. Polyester's superior mechanical and physical qualities have led to its widespread use as a technical textile and garment material in the form of fibers, films, and plastics. Its limited versatility in terms of end use has been caused by its poor surface properties as the hydrophobic nature of polyester surface, roughness, the crystallinity, and lack of dyeability which are the main drawback restricting its use in different textile applications especially during wet treatments unlike natural fibers. In order to increase the fabric's hydrophilicity and dyeability, the surface of a polyester fabric was altered in this study using atmospheric pressure plasma treatment with atmospheric plasma jet and dielectric barrier discharge (APJ-DBD) technology in air. The primary obstacles in making dielectric barrier discharge (DBD) plasma treatment suitable for industrial purposes are the extended duration of treatment and the utilization of elevated voltage levels. The combination between the atmospheric plasma jet and the dielectric barrier discharge reduces the optimal treatment time to 1 min and the applied voltage to 3.3 kV. After being exposed to oxygen plasma species for a brief period of time (between 30 and 300 s), and were analyzed using an X-ray diffraction machine, an X-ray photoelectron spectroscopy (XPS), static contact angle, and a scanning electron microscope (SEM) to investigate changes in the morphology and chemical nature of the surface, respectively. Fabric wettability increased as a result of plasma treatment, which also increased the fabric's surface roughness, as demonstrated by SEM and X-ray diffraction. The contact angle decreases by increasing the treatment time. The dyeability of untreated and plasma-treated samples was examined with respect to washing, rubbing, perspiration, sublimation, and light fastness. Additionally, color strength was examined. Adequately, compared to the untreated fabric, polyester treated with plasma showed improved dyeing performances. The technical reactivity of poly (ethylene-terephthalate) (PET) fabrics was found to be effectively increased by atmospheric air plasma treatment, creating new avenues for surface modification in light of the expanding environmental and energy-saving concerns.

Plasma atomic layer etching of ruthenium by oxygen adsorption-removal cyclic process

Ruthenium (Ru) is a next-generation metal interconnect material, and the demand for precise etching is on the rise. This study explores anisotropic atomic layer etching (ALE) of Ru, utilizing various oxygen adsorption methods (O radical, oxygen plasma, or O2 molecule) and two types of plasma sources: inductively coupled plasma (ICP) and ion beam source. Through ICP ALE, an etch per cycle (EPC) of ∼ 1.5 Å/cycle was achieved using oxygen plasma for adsorption. For ion beam ALE, EPC values of ∼ 0.8 Å/cycle were obtained using oxygen radical, and ∼ 0.4 Å/cycle through physisorption using oxygen molecule without plasma generation. The higher EPC with the ICP ALE was attributed to spontaneous etching during oxygen adsorption during the oxygen plasma generation. Conversely, the lower EPC with ion beam ALE during oxygen adsorption using O2 molecule without plasma generation resulted from nonuniform oxidation of Ru during the adsorption step. Among the three ALE methods, optimal Ru ALE with 100 % ALE synergy was achieved with ion beam ALE, likely due to the absence of ion bombardment during oxygen adsorption and the precise Ar+ ion energy for removing RuOx formed on the surface.

Hybrid Silicon-Organic Methacrylate Monomers and Hyperbranched Polymers that Override the Ohnishi Parameter for Oxygen Plasma Etch Resistance

Hybrid Silicon-Organic Methacrylate Monomers and Hyperbranched Polymers that Override the Ohnishi Parameter for Oxygen Plasma Etch Resistance

Digital etching of AlGaN/GaN heterostructures with GaN cap using inductively coupled oxygen plasma process combined with wet chemical treatment

In this work, AlGaN with a GaN cap has been etched in a cyclical process with ICP-RIE O2 plasma oxidation and wet etching in dilute HCl. The oxygen plasma ICP-RIE etching of the AlGaN at an ICP plasma power of 200 W and radio frequency bias power of 100 W led to an etch depth of ∼1.5 nm per digital cycle with increased surface roughness. The AlGaN remained unaffected by the wet etching process alone without any ICP-RIE O2 plasma oxidation, maintaining a surface roughness similar to that of the substrate. AlGaN was etched to a depth of ∼12 nm after six cycles of digital etching with an etch rate of 1.9–2.1 nm/cycle showing an improved surface roughness. The XPS analysis at each stage of the etching process reveals that the O2 plasma oxidation initially oxidizes the GaN cap and the AlGaN layer and is later effectively removed by the HCl solution. The digital etching method has proven effective in controlling etch depth and surface roughness, which are needed to fabricate AlGaN high electron mobility transistors.

Improving photodetection response time of ReS2 devices through double-sided oxidation

Response time is a crucial factor limiting the performance of two-dimensional material-based photodetectors. The underlying mechanisms of response have recently garnered significant attention in the ongoing research. Supported ReS2 on substrates has been found to be predominantly governed by the photofloating gate effect, known to be slower compared to photoelectric effects. In this study, we present findings demonstrating suspended ReS2 devices. Removing the substrate results in a substantial enhancement in optical response by an order of magnitude compared to substrate-supported devices. Deep trap states induced by inherent defects are identified as the primary contributors to prolonged response times. Engineering these ReS2 trap states through defect manipulation can significantly improve response times. Here, we effectively modulate the response speed of ReS2 through gentle oxygen plasma treatments. The response speed of ReS2 is improved by two orders of magnitude. Under the optimal processing conditions of 50 W, 30 Pa, and 10 s, we observed rising and falling response times of 45 and 106 ms, respectively, under illumination at a wavelength of 637 nm. Additionally, we demonstrate that the input–output characteristic of photocurrent provides valuable insights into the underlying opto-physical processes responsible for generating photocurrent.

Polycaprolactone scaffold surface modification with soft X-ray/extreme ultraviolet (SXR/EUV) radiation and low-temperature oxygen and nitrogen plasma for biomedical applications

Modification of the surfaces of polymeric scaffolds is often required to make the material suitable for specific tissue engineering applications. Physico-chemical properties of scaffolds can be altered using various methods, such as plasma treatment, laser processing, chemical modifications, grafting with nanoparticles, or surface coating. In this paper physico-chemical modification of polycaprolactone (PCL) surface fibers was performed by exposing PCL samples to simultaneous soft X-ray/extreme ultraviolet (SXR/EUV) radiation and low-temperature, SXR/EUV-induced, nitrogen, and oxygen plasmas. The physical and chemical changes on modified PCL surfaces were examined using a scanning electron microscope and X-ray photoelectron spectroscopy, respectively. The effects of physico-chemical scaffold surface changes were verified with biological tests, i.e., MTT assay and immunofluorescence on murine osteoblast cell line (7F2). It was found that exposure of scaffolds to ionizing radiation and low-temperature plasmas induced strong chemical changes on their surface, i.e., appearance of various new chemical groups. Also, smoothing of the surface of PCL fibers, i.e., disappearance or significant reduction of the size of micropores on their fibers was also observed. Increased viability and adhesion of 7F2 osteoblasts on modified PCL samples after 24 h cell culture compared to non-treated PCL was also confirmed.Graphical abstract

Self-powered epitaxial graphene/SiC-C heterojunction UV photodetector

In this paper, local oxygen plasma treatment of SiC carbon surface epitaxial graphene (EG/SiC-C) samples was carried out by using an oxygen plasma processor. Some vacancy defects were introduced into the graphene, and the electronic structure of the graphene was regulated. After oxygen plasma treatment, the work function of EG/SiC-C increased, and the doping type gradually changed to P-type. Finally, a self-powered epitaxial graphene (EG)/SiC heterojunction UV photodetector with spot position response characteristics was prepared by reasonable device structure design.

Preparation and Modeling of Graphene Bubbles to Obtain Strain-Induced Pseudomagnetic Fields.

It has been both theoretically predicted and experimentally demonstrated that strain can effectively modulate the electronic states of graphene sheets through the creation of a pseudomagnetic field (PMF). Pressurizing graphene sheets into bubble-like structures has been considered a viable approach for the strain engineering of PMFs. However, the bubbling technique currently faces limitations such as long manufacturing time, low durability, and challenges in precise control over the size and shape of the pressurized bubble. Here, we propose a rapid bubbling method based on an oxygen plasma chemical reaction to achieve rapid induction of out-of-plane deflections and in-plane strains in graphene sheets. We introduce a numerical scheme capable of accurately resolving the strain field and resulting PMFs within the pressurized graphene bubbles, even in cases where the bubble shape deviates from perfect spherical symmetry. The results provide not only insights into the strain engineering of PMFs in graphene but also a platform that may facilitate the exploration of the strain-mediated electronic behaviors of a variety of other 2D materials.

Evolution of the Surface Wettability of Vertically Oriented Multilayer Graphene Sheets Deposited by Plasma Technology.

Carbon deposits consisting of vertically oriented multilayer graphene sheets on metallic foils represent an interesting alternative to activated carbon in electrical and electrochemical devices such as super-capacitors because of the superior electrical conductivity of graphene and huge surface-mass ratio. The graphene sheets were deposited on cobalt foils by plasma-enhanced chemical vapor deposition using propane as the carbon precursor. Plasma was sustained by an inductively coupled radiofrequency discharge in the H mode at a power of 500 W and a propane pressure of 17 Pa. The precursor effectively dissociated in plasma conditions and enabled the growth of porous films consisting of multilayer graphene sheets. The deposition rate varied with time and peaked at 100 nm/s. The evolution of surface wettability was determined by the sessile drop method. The untreated substrates were moderately hydrophobic at a water contact angle of about 110°. The contact angle dropped to about 50° after plasma treatment for less than a second and increased monotonously thereafter. The maximal contact angle of 130° appeared at a treatment time of about 30 s. Thereafter, it slowly decreased, with a prolonged deposition time. The evolution of the wettability was explained by surface composition and morphology. A brief treatment with oxygen plasma enabled a super-hydrophilic surface finish of the films consisting of multilayer graphene sheets.

Low-Cost Preparation of Diamond Nanopillar Arrays Based on Polystyrene Spheres.

Diamond nanopillar arrays can enhance the fluorescence collection of diamond color centers, playing a crucial role in quantum communication and quantum sensing. In this paper, the preparation of diamond nanopillar arrays was realized by the processes of polystyrene (PS) sphere array film preparation, PS sphere etching shrinkage control, tilted magnetron sputtering of copper film, and oxygen plasma etching. Closely aligned PS sphere array films were prepared on the diamond surface by the gas-liquid interfacial method, and the effects of ethanol and dodecamethylacrylic acid solutions on the formation of the array films were discussed. Controllable reduction of PS sphere diameter is realized by the oxygen plasma etching process, and the changes of the PS sphere array film under the influence of etching power, bias power, and etching time are discussed. Copper antietching films were prepared at the top of arrayed PS spheres by the tilted magnetron sputtering method, and the antietching effect of copper films with different thicknesses was explored. Diamond nanopillar arrays were prepared by oxygen plasma etching, and the effects of etching under different process parameters were discussed. The prepared diamond nanopillars were in hexagonal close-rowed arrays with a spacing of 800 nm and an average diameter of 404 nm, and the spacing, diameter, and height could be parametrically regulated. Raman spectroscopy and photoluminescence spectroscopy detection revealed that the prepared diamond nanopillar array still maintains polycrystalline diamond properties, with only a small amount of the graphite phase appearing. Moreover, the prepared diamond nanopillar array can enhance the photoluminescence of diamond color centers by approximately 2 times. The fabrication method of diamond nanopillar array structures described in this article lays the foundation for quantum sensing technology based on diamond nanostructures.