E. Bertran

Wettability, ageing and recovery process of plasma-treated polyamide 6

The wetting properties of polyamide 6 rods treated with radiofrequency (RF) low-temperature plasma (LTP) using three different non-polymerizing gases (air, nitrogen and water vapour) were determined using the Wilhelmy contact-angle technique. Information on the acidic or basic nature of the ionizable groups generated on the rod surface was obtained using contact-angle titration. The wettability obtained depends on the plasma gas used, and it tends to decrease with time elapsed after the treatment when the samples are kept in an air environment. However, the wettability can be recovered by immersion of the aged samples in water. The degree of recovery depends on the plasma gas used and the highest recovery was obtained with water vapour plasma treated samples. Both ageing and recovery behaviour can be attributed to the reorganisation of hydrophilic groups which tend to reversibly migrate or orient towards the bulk phase depending on the storage conditions, although other factors can also have influence.

In situ spectroellipsometric study of the nucleation and growth of amorphous silicon

A detailed in situ spectroellipsometric analysis of the nucleation and growth of hydrogenated amorphous silicon (a:Si:H) is presented. Photoelectronic quality a‐Si:H films are deposited by plasma‐enhanced chemical vapor deposition on smooth metal (NiCr alloy) and crystalline silicon (c‐Si) substrates. The deposition of a‐Si:H is analyzed from the first monolayer up to a final thickness of 1.2 μm. In order to perform an improved analysis, real time ellipsometric trajectories are recorded, using fixed preparation conditions, at various photon energies ranging from 2.2 to 3.6 eV. The advantage of using such a spectroscopic experimental procedure is underlined. New insights into the nucleation and growth mechanisms of a‐Si:H are obtained. The nucleation mechanism on metal and c‐Si substrates is very accurately described assuming a columnar microstructural development during the early stage of the growth. Then, as a consequence of the incomplete coalescence of the initial nuclei, a surface roughness at the 10–...

Shrink-resistance and wetting properties of keratin fibres treated by glow discharge

The influence of the gas type, air or nitrogen, and the treatment time in an RF glow discharge treatment on the shrink resistance properties of knitted wool fabric and wetting properties of keratin fibres were studied. Wetting properties were determined by means of contact angle measurements on single keratin fibres. This method allows measuring accurately the influence of the plasma gas type and treatment time on fibre hydrophilicity, and its modification with the time elapsed after plasma treatment. The modification of the surface properties should be taken into account, especially, when a biopolymer after-treatment is applied to achieve wool shrink resistance. Surface chemical changes were studied by means of XPS. Topographical changes in the wool fibre surface were observed by scanning electron microscopy (SEM) and surface damage was evaluated by means of the Herbig sac formation. Both air and nitrogen plasma treatments impart shrink resistance to wool fabric and hydrophilic properties to the keratin fibres. Even short exposure times are found to be enough to decrease drastically the advancing water contact angle and, therefore, to increase the shrink resistance effect. Slight differences were observed between the air and nitrogen plasma treatments. The time elapsed after the plasma treatment promotes an increase of the advancing contact angle and a decrease of chitosan adsorption. The plasma treatments studied here modify chemically the epicuticle but it is not removed.

Electrochromic behaviour of nickel oxide thin films deposited by thermal evaporation

Within an all-solid inorganic layout for an electrochromic device with tungsten trioxide acting as main electrochromic layer, there are a few possible electrochromic complementary materials that can act as the ionic storage layer, and among them nickel oxide has always attracted considerable interest. We analysed nickel oxide deposited by thermal evaporation to test the suitability of such a layer for use in an all-solid inorganic electrochromic device. Samples were analysed with X-ray photoelectron spectroscopy and electrochemical techniques, cyclic voltammetry and chronoamperometry with simultaneous monitoring of the optical properties of the samples. The characterisation deals with the activation potential ranges, the amount of inserted charge, colouration efficiency and optical and electrical compatibility with the tungsten trioxide layers. All these analyses provided criteria for the relation between the electrochromic properties of the thin films of nickel oxide and the deposition parameters employed, and opened a way to obtain cost-effective all-solid inorganic electrochromic devices.

Atomic structure of the nanocrystalline Si particles appearing in nanostructured Si thin films produced in low-temperature radiofrequency plasmas

Nanostructured Si thin films, also referred as polymorphous, were grown by plasma-enhanced chemical vapor deposition. The term “polymorphous” is used to define silicon material that consists of a two-phase mixture of amorphous and ordered Si. The plasma conditions were set to obtain Si thin films from the simultaneous deposition of radical and ordered nanoparticles. Here, a careful analysis by electron transmission microscopy and electron diffraction is reported with the aim to clarify the specific atomic structure of the nanocrystalline particles embedded in the films. Whatever the plasma conditions, the electron diffraction images always revealed the existence of a well-defined crystalline structure different from the diamondlike structure of Si. The formation of nanocrystallinelike films at low temperature is discussed. A Si face-cubic-centered structure is demonstrated here in nanocrystalline particles produced in low-pressure silane plasma at room temperature.

Growth of hydrogenated amorphous carbon films in pulsed d.c. methane discharges

Abstract We report the preparation of hydrogenated amorphous carbon (a-C:H) films from asymmetrical bipolar pulsed d.c. methane discharges. The films were deposited at 10 Pa of pressure on c-Si substrates placed onto an electrode powered by a pulsed d.c. generator. The asymmetrical bipolar pulsed d.c. voltage waveform consisted of a fixed positive pulse amplitude of 40 V followed by a variable negative pulse whose peak amplitude was varied from −400 up to −1400 V. Pulse frequencies of 100, 125, 150 and 200 kHz were used at a constant positive pulse time of 2 μs. In addition, a series of a-C:H samples were grown from r.f. capacitive discharges at bias voltages from −200 to −800 V. Pulsed d.c. a-C:H films 1-μm-thick were deposited at growth rates up to 60 nm/min and with internal compressive stress values between 1 and 1.5 GPa. Fourier transform-infrared and Raman analyses revealed the diamond-like character of the films. The effects of pulse parameters on the growth and structural properties of the films are discussed and compared to those of films obtained by conventional r.f. plasma-enhanced chemical vapour deposition.

Size dependence of energy gaps in small carbon clusters: the origin of broadband luminescence

Abstract The visible broadband luminescence from carbon-related films has recently been attributed to the band-tail states caused by the variations in the energy gap of individual sp 2 carbon clusters due to their difference in size and/or shape. In this paper, these band-tail states are classified into two parts: localized and confined. The localized states result from the structural deviation from graphite-like configuration, and the associated luminescence may be described by using the conventional theory for amorphous materials. The confined states are generated due to the existence of stable graphite-like local structures with various sizes and are the main factor for giving efficient, room-temperature luminescence. Our calculations of a series of small hexagonal carbon clusters with first-principle and semi-empirical methods demonstrate that the energy-gap distribution, due to the difference in size, is considerably broad, which may explain the broadband feature of luminescence. Calculations for some tetrahedral clusters were also made for comparison.

Ellipsometric study of a‐Si:H thin films deposited by square wave modulated rf glow discharge

Thin films of hydrogenated amorphous silicon (a‐Si:H), deposited by square wave modulated (SQWM) rf silane discharges, have been studied through spectroscopic and real time phase modulated ellipsometry. The SQMW films obtained at low mean rf power density (19 mW/cm2) have shown smaller surface roughness than those obtained in standard continuous wave (cw) rf discharges. At higher rf powers (≥56 mW/cm2), different behaviors depending on the modulating frequency have been observed. On the one hand, at low modulating frequencies (<40 Hz), the SQWM films have shown a significant increase of porosity and surface roughness as compared to cw samples. On the other, at higher modulating frequencies, the material density and roughness have been found to be similar in SQWM and cw films. Furthermore, the deposition rate of the films show more pronounced increases with the modulating frequency as the rf power is increased. Experimental results are discussed in terms of plasma negative charged species which can be rela...

Optical properties of co-evaporated CuInSe2 thin films

Thin films of CuInSe2 within a wide composition range around stoichiometry have been deposited by Cu, In and Se co-evaporation. Their optical properties in the near-infrared have been studied in relation to the composition and the deposition process parameters. The refractive index and the absorption coefficient below the absorption edge, depend on the Cu-In percentages ratio and show a minimum at stoichiometry. Moreover, the refractive index increases with the deposition temperature. Beyond the absorption edge the absorption is due to an allowed direct transition and a forbidden direct transition with gap energies around 1.0 and 1.2 eV, respectively. The values of the optical gaps depend on the Cu-In percentages ratio and show a minimum at stoichiometry. These dependences have been correlated with the variations of the crystalline lattice constant with the Cu-In ratio.

Functionalization of carbon nanotubes by water plasma

Multiwall carbon nanotubes grown by plasma enhanced chemical vapour deposition were functionalized by H(2)O plasma treatment. Through a controlled functionalization process of the carbon nanotubes (CNTs) we were able to modify and tune their chemical reactivity, expanding the range of potential applications in the field of energy and environment. In particular, different oxygen groups were attached to the surfaces of the nanotubes (e.g. carboxyl, hydroxyl and carbonyl), which changed their physicochemical properties. In order to optimize the main operational parameters of the H(2)O plasma treatment, pressure and power, a Box-Wilson experimental design was adopted. Analysis of the morphology, electrochemical properties and functional groups attached to the surfaces of the CNTs allowed us to determine which treatment conditions were suitable for different applications. After water plasma treatment the specific capacitance of the nanotubes increased from 23 up to 68 F g(-1) at a scan rate of 10 mV s(-1).