Plasma technologies have been utilized to improve the surface properties of fibres in many applications from textiles to fibre-reinforced composites since the 1960s. This review discusses the feasibility and characteristics of plasma technologies applied to fibre-reinforced polymer composites. The influence of various plasma treatments on the chemical and mechanical properties of different fibres as well as fibre-reinforced composites is described. The difference between polymer fibres and carbon fibres is emphasized to achieve good bonding between fibres and matrices and to enhance the mechanical properties of the composites. More sophisticated technologies such as microwave plasma and plasma-initiated graft polymerization are also discussed to highlight very recent developments.

Application of plasma technologies in fibre-reinforced polymer composites: a review of recent developments

In this paper, we present a study on the surface modification of polyethyleneterephthalate (PET) polymer by plasma treatment. The samples were treated by nitrogen and oxygen plasma for different time periods between 3 and 90 s. The plasma was created by a radio frequency (RF) generator. The gas pressure was fixed at 75 Pa and the discharge power was set to 200 W. The samples were treated in the glow region, where the electrons temperature was about 4 eV, the positive ions density was about 2 × 1015 m−3, and the neutral atom density was about 4 × 1021 m−3 for oxygen and 1 × 1021 m−3 for nitrogen. The changes in surface morphology were observed by using atomic force microscopy (AFM). Surface wettability was determined by water contact angle measurements while the chemical composition of the surface was analyzed using XPS. The stability of functional groups on the polymer surface treated with plasma was monitored by XPS and wettability measurements in different time intervals. The oxygen-plasma-treated samples showed much more pronounced changes in the surface topography compared to those treated by nitrogen plasma. The contact angle of a water drop decreased from 75° for the untreated sample to 20° for oxygen and 25° for nitrogen-plasma-treated samples for 3 s. It kept decreasing with treatment time for both plasmas and reached about 10° for nitrogen plasma after 1 min of plasma treatment. For oxygen plasma, however, the contact angle kept decreasing even after a minute of plasma treatment and eventually fell below a few degrees. We found that the water contact angle increased linearly with the O/C ratio or N/C ratio in the case of oxygen or nitrogen plasma, respectively. Ageing effects of the plasma-treated surface were more pronounced in the first 3 days; however, the surface hydrophilicity was rather stable later. Copyright © 2008 John Wiley & Sons, Ltd.

Surface modification of polyester by oxygen- and nitrogen-plasma treatment

Polytetrafluoroethylene (PTFE) was treated in a low-power plasma using a series of feed gases (O 2 , Ar, N 2 and NH 3 ) and the resulting surface modifications were evaluated by x-ray photoelectron spectroscopy, static secondary ion mass spectroscopy, dynamic contact angle measurements and atomic force microscopy. All plasma treatments caused light etching, but the nature and extent of chemical modification varied considerably. Fluorine depletion of the surface was affected most efficiently by Ar and least effectively by O 2 plasma. New functionalities were introduced to the surface either from plasma derivatives of the feed gases or by post-treatment exposure to moist air; Ar, N 2 and NH 3 were more effective than O 2 in this respect. The wettability of virgin and plasma-treated materials in phosphate-buffered saline solution (PBS) and 1-bromonaphthalene was studied, and the observations are discussed in a framework that correlates contact-angle hysteresis with surface chemistry in a semi-quantitative manner. In Part II of this work, further changes of the surface chemistry and wettability of virgin and plasma-treated materials arising due to storage in PBS or air are described.

Plasma modification of PTFE surfaces. Part I: Surfaces immediately following plasma treatment

Carbon fibers and composites with epoxy resins: Topography, fractography and interphases

Atmospheric pressure plasma processing has attracted significant interests over decades due to its usefulness and a variety of applications. Adhesion improvement of polymer surfaces is among the most important applications of atmospheric pressure plasma treatment. Reflecting recent significant development of the atmospheric pressure plasma processing, this work presents its fundamental aspects, applications, and characterization techniques relevant to adhesion.

Atmospheric Pressure Plasma Processing for Polymer Adhesion: A Review

This paper describes the effects that a low-power plasma (< 1 W) has on the chemistry, topography and surface energy of polyethylene (PE) film. The gases used for treating the film were air and nitrogen. The plasma cell was attached directly to the preparation chamber of an x-ray photoelectron spectrometer, enabling the immediate effects of the plasma on the chemical nature of the films to be monitored. Significant amounts of chemical functionality were introduced onto the surface using both plasmas even after a few seconds of treatment. Carbon/oxygen functionality dominates surfaces treated with an air plasma. Nitrogen plasma treatment, as expected, introduced amines, imines and amides. Exposing the treated surfaces to air results in oxygen adsorption, the amount of oxygen pick-up being time dependent. This ageing of the treated polymer films is thought to occur via two processes: short-term hydrolysis of the amines and gradual oxidation of the polymer chain itself. The topographical changes were studied using atomic force microscopy, which was performed after the films bad been exposed to air. Both plasmas caused the polymer surface to roughen, with nitrogen plasma treatment having a more pronounced effect. The surface energy of the film was increased from 37 dyn cm −1 (untreated) to 47 and 46 dyn cm −1 after 20 s of exposure to air and nitrogen plasmas, respectively. After 1 min of treatment, the polar surface energy component of the film treated with a nitrogen plasma (12 dyn cm −1 ) was much higher than that treated with an air plasma (7 dyn cm −1 ). This is supported by the XPS results in that the concentration of chemical groups introduced onto the surface after nitrogen plasma treatment was greater than that for air. The greater changes in polymer surface properties observed for nitrogen plasma treatment were not reflected in the values obtained for the level of polymer/metal adhesion. Only air plasma-treated samples showed significant improvement in the adhesion between polyethylene and alumininm and we conclude that the presence of oxygencontaining functional groups plays a major role in this improvement

Effects of low‐power plasma treatment on polyethylene surfaces

Ammonia plasmas produced in a helical resonator have been investigated using an energy-selective mass spectrometer and an r.f.-compensated Langmuir probe. The effect of processing parameters on the plasma composition and ion energy distributions have been examined. The dominant ion present in the plasma was found to be NH 4 + , which varied in concentration between 95% and 65%, dependent upon operating conditions. Similarly, by relatively small variations in processing parameters it was possible to vary the NH 3 + ion concentration between 1.7 and 31%. In addition, no radicals (NH 2 . , NH . or N . ) were detected using threshold ionization mass spectroscopy. Polytetrafluoroethylene (PTFE) samples were treated under a variety of different plasma conditions, and the chemical changes induced were studied by in situ XPS. Defluorination was observed to be greater under conditions that yield low ion energies or high concentrations of NH 3 + ions. Conditions giving rise to significant concentrations of NH 3 + ions result in the production of NH 3 + F - groups. Evidence is provided suggesting that NH 3 + ions are much more reactive with PTFE surfaces than NH 4 + ions

Ammonia Plasma Treatment of PTFE Under Known Plasma Conditions

A low-power plasma treatment has been adapted to work on a pilot plant scale to continuously treat a tow of carbon fibres. This treatment successfully increases fibre-resin adhesion to levels comparable it not higher than those obtained by commercial electrochemical treatments. One advantage is that the plasma treatment does not appear to affect the tensile properties of the fibre, unlike the electrochemical oxidation. We have also shown that the chemical groups introduced during air plasma treatment play a significant role in fibre-resin adhesion whereas those introduced by electrochemical oxidation do not. A possible explanation for this is that plasma treatments introduce chemical groups onto the immediate surface of the fibres that have the potential to react with the resin, whereas electrochemical oxidation occurs predominantly at the edge sites and proceeds into the sublayers of the fibre. The vast majority of the functional groups are therefore inaccessible to the resin. This type of plasma treatment, however, is unlikely to remove all of the weakly bound layers as in the case of electrochemical treatment because the sputtering capability of the plasma is very low. The tact that these conclusions can be drawn from both the single-fibre fragmentation test and the short-beam shear test is encouraging and goes to prove that both these tests are suitable for looking at trends in fibre-resin adhesion

Effect of low‐power air plasma treatment on the mechanical properties of carbon fibres and the interfacial shear strength of carbon fibre—epoxy composites

X-ray photoelectron spectroscopy (XPS) and static secondary ion mass spectrometry (SIMS) have been used to determine the chemical changes observed as a result of interactions between carbon fibre surfaces and epoxy resins. A comparison has been made between untreated, commercially treated and air plasma treated carbon fibres. Both positive and negative static SIMS results indicated the presence of nitrogen and oxygen containing fragments as a result of air plasma treatment, the spectra from commercially treated fibres were dominated by contaminants. Fibres were then sized in the monofunctional epoxy resin, 1,2-epoxy-3-phenoxypropane, and further analysis carried out to determine the chemical nature of the fibre-resin interface. Angle resolved XPS was used to confirm the presence of a layer of resin. Positive ion fragments from static SIMS data have been identified as species which have been formed as a result of the epoxy molecule chemically reacting with species on the fibre surface. Surface energy measurements have also been recorded and it is shown that the polar component of surface energy is greatly increased as a result of surface treatment. This increase is much greater for air plasma treated fibres than for commercially treated fibres. It is proposed that air plasma treatment of carbon fibres increases the interfacial adhesion in carbon fibre/epoxy composites, by the introduction of functional groups which form chemical bonds with the epoxy resin.

Study of the interaction of carbon fibre surfaces with a monofunctional epoxy resin

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Papers

Effects of low‐power plasma treatment on polyethylene surfaces

Ammonia Plasma Treatment of PTFE Under Known Plasma Conditions

Effect of low‐power air plasma treatment on the mechanical properties of carbon fibres and the interfacial shear strength of carbon fibre—epoxy composites

Study of the interaction of carbon fibre surfaces with a monofunctional epoxy resin