Influence of oxygen plasma treatment parameters on poly(vinylidene fluoride) electrospun fiber mats wettability

Electrospun poly(vinylidene fluoride) (PVDF) fiber mats find applications in an increasing number of areas, such as battery separators, filtration and detection membranes, due to their excellent properties. However, there are limitations due to the hydrophobic nature and low surface energy of PVDF. In this work, oxygen plasma treatment has been applied in order to modify the surface wettability of PVDF fiber mats and superhydrophilic PVDF electrospun membranes have been obtained. Further, plasma treatment does not significantly influences fiber average size (~400 ± 200 nm), morphology, electroactive -phase content (~80-85%) or the degree of crystallinity (Xc of 42 ± 2%), allowing to maintain the excellent physical-chemical characteristics of PVDF. Plasma treatment mainly induces surface chemistry modifications, such as the introduction of oxygen and release of fluorine atoms that significantly changes polymer membrane wettability by a reduction of the contact angle of the polymer fibers and an overall decrease of the surface tension of the membranes.

Erratum: Influence of oxygen plasma treatment parameters on poly(vinylidene fluoride) electrospun fiber mats wettability

Electrospun poly(vinylidene fluoride) (PVDF) fiber mats find applications in an increasing number of areas, such as battery separators, filtration and detection membranes, due to their excellent properties. However, there are limitations due to the hydrophobic nature and low surface energy of PVDF. In this work, oxygen plasma treatment has been applied in order to modify the surface wettability of PVDF fiber mats and superhydrophilic PVDF electrospun membranes have been obtained. Further, plasma treatment does not significantly influences fiber average size (~400 ± 200 nm), morphology, electroactive -phase content (~80-85%) or the degree of crystallinity (Xc of 42 ± 2%), allowing to maintain the excellent physical-chemical characteristics of PVDF. Plasma treatment mainly induces surface chemistry modifications, such as the introduction of oxygen and release of fluorine atoms that significantly changes polymer membrane wettability by a reduction of the contact angle of the polymer fibers and an overall decrease of the surface tension of the membranes.

Oxygen plasma treatment of sisal fibers and polypropylene: Effects on mechanical properties of composites

Polypropylene powder and sisal fibers were oxygen plasma treated, and the mechanical properties of their composites were tested. Two main effects were investigated: the incorporation of oxygen polar groups in the polypropylene surface and the surface degradation and chain scission of both polypropylene and sisal fibers. Prior to these treatments, three reactor configurations were tested to investigate the best condition for both effects to occur in PP film. Results showed that polypropylene-cellulose adhesion forces are about an order of magnitude higher for PP film treatments at 13.56 MHz than at 40 kHz owing to much higher chain scission at lower frequencies, although it probably also occurs at high frequency and high power. Polypropylene powder treated with oxygen plasma in optimum conditions for polar group incorporation did not result in improvement in any composite mechanical property, probably owing to the polymer melting. Sisal fibers and PP powder treated In conditions of surface degradation did not improve flexural or tensile properties but resulted in higher impact resistance, comparable to the improvement obtained with the addition of compatibilizer.

Controlled surface nanotopography and oxygen plasma treatment of PEEK to improve cellular response

Poly(aryl-ether-ether-ketone) (PEEK) is a semi crystalline polymer which exhibits properties that make it an attractive choice for use as an implant material. It displays natural radiolucency, and MRI compatibility, as well as good chemical and sterilization resistance, both of which make it of particular interest in orthopaedic implants. However, PEEK has demonstrated poor cellular adhesion both in vitro and in vivo. This is problematic as implant surfaces that do not develop a layer of adhesive cells are at risk of undergoing fibrous encapsulation, which in turn leads to lack of a strong interface between the implant device and the patient tissue, which can in turn lead to failure of the implant and revision surgery . As incorporating nanotopography into a polymer surface has been demonstrated to be able to direct the differentiation behaviour of stem cells, a possible solution to PEEKs underlying issues with poor cellular response would be to incorporate specific nanoscale topography into the material surface through injection moulding, and then analysing if this is a viable method for addressing PEEKs issues with cellular response. In addition to nanoscale topography, the experimental PEEK surfaces were treated with oxygen plasma to address the underlying cytophobicity of the material. As this type of treatment has been documented to be capable of etching the PEEK surface, experiments were carried out to quantify the effect of this treatment, both on the ability of cells to adhere to the PEEK surface, as well as the effect it has upon the nanotopography present at the PEEK surface. The results demonstrated that there were a range of plasma treatments which would significantly improve the ability of cells to adhere to the PEEK surface without causing unacceptable damage to the nanotopography. Three different types of cells with osteogenic capacity were tested with the PEEK surfaces to gauge the ability of the topography to alter their behaviour: SAOS-2, osteoprogenitors and 271+ MSCs. Due to PEEKs material properties (it is non transparent, exhibits birefringence and is strongly autofluorescent) a number of histological techniques were used to investigate a number of different stages that take place in osteogenesis. The different cell types did display slightly different responses to the topographies. The SAOS-2 cells cultured on surfaces that had been plasma treated for 2 minutes at 200W had statistically significantly higher levels of von Kossa staining on the NSQ surface compared to the planar surface, and the same experiment employing alizarin red staining, showed a statistically significantly lower level of staining on the SQ surface compared to the planar surface. Using primary osteoprogenitor cells designed to look into if whether or not the presence of nanotopography effected the osteogenic response of these cells, we saw a lack of statistically significant difference produced by the surfaces investigated. By utilising HRP based immunostaining, we were able to investigate, in a quantitative fashion, the production of the two osteogenic markers osteopontin and osteocalcin by cells. When stained for osteocalcin, the SQ nanotopography had total percentage of the surface with stained material, average area and average perimeter all statistically significantly lower than the planar surface. For the cells that were stained for osteopontin, the SQ nanotopgraphy had a total percentage of the surface with stained material, average area and average perimeter all highly statistically significantly lower than those of the planar surface. Additionally, for this marker the NSQ nanotopography had average areas and average perimeters that were highly significantly higher than those of the planar surface. There were no significant differences for any of the values investigated for the 271+ MSC’s When plasma treatment was varied, the SAOS-2 cells demonstrated an overall trend i.e. increasing the energy of plasma treatment in turn leads to an increase in the overall percentage of staining. A similar experiment employing stem cells isolated from human bone marrow instead of SAOS-2 cells showed that for polycarbonate surfaces , used as a control, mineralization is statistically significantly higher on the NSQ nanopattern compared to the planar surface, whereas on the PEEK surfaces we observe the opposite trend i.e. the NSQ nanotopography having a statistically significantly lower amount of mineralization compared to the planar surface at the 200W 2min and 30W 1min plasma treatments. The standout trend from the PEEK results in this experiment was that the statistically significant differences on the PEEK substrates were clustered around the lower energy plasma treatments, which could suggest that the plasma treatment disrupted a function of the nanotopograhy which is why, as the energy increases, there are less statistically significant differences between the NSQ nanotopography and the Planar surface This thesis documents the response of a number of different types of cells to specific nanoscale topographies incorporated into the PEEK surface which had been treated with oxygen plasma. It outlines the development of a number of histological methods which measure different aspects of osteogenesis, and were selected to both work with PEEK, and produce quantitative results through the use of Cell Profiler. The methods that have been employed in this body of work would be of interest to other researchers working with this material, as well as those working with similarly autofluorescent materials.

Microbial Decontamination Study of Medicinal Plants by Plasma Treatment

In the present work the microbial decontamination of some medicinal plants by plasma treatment using oxygen gas or a mixture of oxygen and hydrogen peroxide was investigated. The efficiency of the decontamination process was analyzed by the count of heterotropic microorganisms and pathogenic research. The results showed a reduction in the microorganism number such as 3 and 4 logarithmic cycles for ginkgo and artichoke, while it was not efficient for samples containing hard and thick cells, and mucilage, such as guarana and chamomile.

Surface energy increase of oxygen-plasma-treated PET

Prosthetic composite is a widely used biomaterial that satisfies the criteria for application as an organic implant without adverse reactions. Polyethylene therephthalate (PET) fiber-reinforced composites have been used because of the excellent cell adhesion, biodegradability and biocompatibility. The chemical inertness and low surface energy of PET in general are associated with inadequate bonds for polymer reinforcements. It is recognized that the high strength of composites, which results from the interaction between the constituents, is directly related to the interfacial condition or to the interphase. A radio frequency plasma reactor using oxygen was used to treat PET fibers for 5, 20, 30 and 100 s. The treatment conditions were 13.56 MHz, 50 W, 40 Pa and 3.33 x 10(-7) m(3)/s. A Rame-Hart goniometer was used to measure the contact angle and surface energy variation of fibers treated for different times. The experimental results showed contact angle values from 47degrees to 13degrees and surface energies from 6.4 x 10(-6) to 8.3 x 10(-6) J for the range of 5 to 100 s, respectively. These results were confirmed by the average ultimate tensile strength of the PET fiber/polymethylmethacrylate (PMMA) matrix composite tested in tensile mode and by scanning electron microscopy. (C) 2003 Elsevier B.V. All rights reserved.

Effect of cold plasma treatment on mechanical properties of PET/PMMA composites

Mechanical strength of polyethylene terephthalate (PET) fibres and polymethyl methacrylate (PMMA) matrix composites were studied with particular interest on the effects of oxygen and argon plasma treated fibres. PET. fibres were treated in a radio frequency plasma reactor using argon or oxygen for different treatment times to increase the interface adhesion. Fibre volume fraction was measured through digital image analysis. Elastic moduli resulted between 3 GPa for untreated to 6 GPa for treated composites. Tensile tests on PET fibres showed that plasma treatment caused a decrease in average tensile strength compared to untreated fibres. Fracture analysis confirmed the increase in interfacial adhesion due to plasma treatment. (c) 2004 Elsevier Ltd. All rights reserved.

Atmospheric plasma treatment of carbon fibers for enhancement of their adhesion properties

Plasma processing of carbon fibers (CFs) is aimed to provide better contact and adhesion between individual plies without decrease in the CF mechanical resistance. This paper deals with surface modification of CFs by an atmospheric pressure dielectric barrier discharge (DBD) for enhancing the adhesion between the CF and the polymeric matrix. The scanning electron microscopy of the treated samples revealed many small particles distributed over entire surface of the fiber. These particles are product of the fiber surface etching during the DBD treatment that removes the epoxy layer covering as-received samples. The alteration of the CF surface morphology was also confirmed by the Atomic force microscopy (AFM), which indicated that the CF roughness increased as a result of the plasma treatment. The analysis of the surface chemical composition provided by X-ray photoelectron spectroscopy showed that oxygen and nitrogen atoms are incorporated onto the surface. The polar oxygen groups formed on the surface lead to the increasing of the CF surface energy. The results of interlaminar shear strength test (short beam) of CFs/polypropylene composites demonstrated a greater shear resistance of the composites made with CFs treated by DBD than the one with untreated fibers. Both the increase in surface roughness and the surface oxidation contribute for the enhancement of CF adhesion properties. © 2012 IEEE.

Solid-state hydrolysis of postconsumer polyethylene terephthalate after plasma treatment

Plasma treatments were applied on the surface of postconsumer polyethylene terephthalate (PET) bottles to increase their wettability and hasten the subsequent hydrolysis process. Sixty-four treatments were tested by varying plasma composition (oxygen and air), power (25-130 W), pressure (50-200 mTorr), and time (1 and 5 min). The best treatment was the one applied in air plasma at 130 W and 50 mTorr for 5 min, as it provided the lowest contact angle, 9.4°. Samples of PET before and after the optimized plasma condition were subjected to hydrolysis at 205°C. Although the treatment changed only a thin surface layer, its influence was evident up to relatively high conversion rates, as the treated samples presented more than 40% higher conversion rates than the untreated ones after 2 h of reaction. Infrared spectroscopy showed that the terephthalic acid obtained from 99% of depolymerization was similar to the commercial product used in PET synthesis. © 2012 Wiley Periodicals, Inc.

Surface characterization of lithium disilicate ceramic after nonthermal plasma treatment

Statement of problem. Surface transformation with nonthermal plasma may be a suitable treatment for dental ceramics, because it does not affect the physical properties of the ceramic material.Purpose. The purpose of this study was to characterize the chemical composition of lithium disilicate ceramic and evaluate the surface of this material after nonthermal plasma treatment.Material and methods. A total of 21 specimens of lithium disilicate (10 mm in diameter and 3 mm thick) were fabricated and randomly divided into 3 groups (n=7) according to surface treatment. The control group was not subjected to any treatment except surface polishing with abrasive paper. In the hydrofluoric acid group, the specimens were subjected to hydrofluoric acid gel before silane application. Specimens in the nonthermal plasma group were subjected to the nonthermal plasma treatment. The contact angle was measured to calculate surface energy. In addition, superficial roughness was measured and was examined with scanning electron microscopy, and the chemical composition was characterized with energy-dispersive spectroscopy analysis. The results were analyzed with ANOVA and the Tukey honestly significant difference test (alpha=.05).Results. The water contact angle was decreased to 0 degrees after nonthermal plasma treatment. No significant difference in surface roughness was observed between the control and nonthermal plasma groups. Scanning electron microscopy and energy-dispersive spectroscopy images indicated higher amounts of oxygen (O) and silicon (Si) and a considerable reduction in carbon (C) in the specimens after nonthermal plasma treatment.Conclusions. Nonthermal plasma treatment can transform the characteristics of a ceramic surface without affecting its surface roughness. A reduction in C levels and an increase in 0 and Si levels were observed with the energy-dispersive spectroscopy analysis, indicating that the deposition of the thin silica film was efficient.

Atmospheric plasma treatment of porous polymer constructs for tissue engineering applications

Porous 3D polymer scaffolds prepared by TIPS from PLGA (53:47) and PS are intrinsically hydrophobic which prohibits the wetting of such porous media by water. This limits the application of these materials for the fabrication of scaffolds as supports for cell adhesion/spreading. Here we demonstrate that the interior surfaces of polymer scaffolds can be effectively modified using atmospheric air plasma (AP). Polymer films (2D) were also modified as control. The surface properties of wet 2D and 3D scaffolds were characterised using zeta-potential and wettability measurements. These techniques were used as the primary screening methods to assess surface chemistry and the wettability of wet polymer constructs prior and after the surface treatment. The surfaces of the original polymers are rather hydrophobic as highlighted but contain acidic functional groups. Increased exposure to AP improved the water wetting of the treated surfaces because of the formation of a variety of oxygen and nitrogen containing functions. The morphology and pore structure was assessed using SEM and a liquid displacement test. The PLGA and PS foam samples have central regions which are open porous interconnected networks with maximum pore diameters of 49 μm for PLGA and 73 μm for PS foams. (Figure Presented) © 2007 Wiley-VCH Verlag GmbH & Co. KGaA.

Sterilization by pure oxygen plasma and by oxygen-hydrogen peroxide plasma: An efficacy study

Plasma is an innovative sterilization method characterized by a low toxicity to operators and patients, and also by its operation at temperatures close to room temperatures. The use of different parameters for this method of sterilization and the corresponding results were analyzed in this study. A low-pressure inductive discharge was used to study the plasma sterilization processes. Oxygen and a mixture of oxygen and hydrogen peroxide were used as plasma source gases. The efficacy of the processes using different combinations of parameters such as plasma-generation method, type of gas, pressure, gas flow rate, temperature, power, and exposure time was evaluated. Two phases were developed for the processes, one using pure oxygen and the other a mixture of gases. Bacillus subtilis var. niger ATCC 9372 (Bacillus atrophaeus) spores inoculated on glass coverslips were used as biological indicators to evaluate the efficacy of the processes. All cycles were carried out in triplicate for different sublethal exposure times to calculate the D value by the enumeration method. The pour-plate technique was used to quantify the spores. D values of between 8 and 3 min were obtained. Best results were achieved at high power levels (350 and 40oW) using pure oxygen, showing that plasma sterilization is a promising alternative to other sterilization methods. (c) 2007 Elsevier B.V. All rights reserved.

Characterization of physical, mechanical and chemical properties of quiscal fibres : the influence of atmospheric DBD plasma treatment

This paper reports the first attempt of characterizing various physical, mechanical and chemical properties of Quiscal fibres, used by the native communities in Chile and investigating the influence of atmospheric dielectric barrier discharge plasma treatment on various properties such as diameter and linear density, fat, wax and impurity%, moisture regain, chemical elements and groups, thermal degradation, surface morphology, etc. According to the experimental observations, Quiscal fibre has lower tenacity than most of the technical grade natural fibres such as sisal, hemp, flax, etc., and plasma treatment at optimum dose improved its tenacity to the level of sisal fibres. Plasma treatment also reduced the amount of fat, wax and other foreign impurities present in Quiscal fibres as well as removed lignin and hemicellulose partially from the fibre structure. Plasma treatment led to functionalization of Quiscal fibre surface with chemical groups, as revealed from attenuated total reflection spectroscopy and also confirmed from the elemental analysis using energy dispersive Xray technique and pH and conductivity measurements of fibre aqueous extract. The wetting behavior of Quiscal fibre also improved considerably through plasma treatment. However, untreated and plasma treated Quiscal fibres showed similar thermal degradation behavior, except the final degradation stage, in which plasma treated fibres showed higher stability and incomplete degradation unlike the untreated fibres. The experimental results suggested that the plasma treated Quiscal fibres, like other technical grade natural fibres, can find potential application as reinforcement of composite materials for various industrial applications.

Characterization of physical, mechanical and chemical properties of quiscal fibres: the influence of atmospheric dbd plasma treatment

This paper reports the first attempt of characterizing several physical, mechanical and chemical properties of Quiscal fibres, usually used by the native communities in Chile and on investigations concerning the influence of atmospheric dielectric barrier discharge (DBD) plasma treatment on various properties such as diameter and linear density, percent of impurity, moisture regain, chemical elements and groups, thermal degradation, surface morphology, among others.

Hyperbaric oxygen therapy treatment for the fixation of implant prosthesis in oncology patients irradiated

doi: 10.1111/j.1741-2358.2012.00636.x Hyperbaric oxygen therapy treatment for the fixation of implant prosthesis in oncology patients irradiated Objectives: This study aimed to present a clinical report of an irradiated oncologic patient who underwent hyperbaric oxygen therapy to be rehabilitated with implant-supported prosthesis. Materials and Methods: A 67-year-old man was admitted at Oral Oncology Center (FOA-UNESP) presenting a lesion on the mouth floor. After clinical evaluation, incisional biopsy and histopathological exam, a grade II squamous cell carcinoma was diagnosed. The patient was subjected to surgery to remove the lesion and partial glossectomy. Afterwards, the radiotherapy, in the left/right cervicofacial area of the supraclavicular fossa, was conducted. After 3 years of the surgery, the patient was submitted to hyperbaric oxygen therapy. Then, four implants were installed in patients mandible. Five months later, an upper conventional complete denture and lower full-arch implant-supported prosthesis were fabricated. Conclusion: The treatment resulted in several benefits such as improving his chewing efficiency, swallowing and speech, less denture trauma on the mucosa and improving his self-esteem.