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The present study deals with the consolidation of an ultra-high performance polymer, the poly(ether ether ketone) (PEEK), for structural applications, using the powder metallurgy (PM) way, and more precisely the Spark Plasma Sintering (SPS) processing. The effects of SPS parameters such as temperature, pressure, and dwell time on density and mechanical properties of PEEK were investigated via a Design of Experiments (DoE). A temperature of 250 °C, a pressure of 40 MPa, and a dwell time of 20 min have been identified as the optimal SPS process parameters. In these conditions, a density of 1.31 g/cm3 was reached and homogeneous mechanical properties in the volume determined by means of compression tests were found with a compressive modulus of 2.75 GPa, a yield strength of 134 MPa, and a maximum compressive strain of 43%. These results are better than those of commercial products obtained by injection molding. The pressure appears to be a significant parameter on PEEK properties and plays positive or negative roles according to the responses of DoE studied. To our knowledge, it is one of the first studies based on the application of the PM techniques for PEEK consolidation showing the possibility to process below its melting point. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017, 134, 44911.

The nitrogen content in tantalum nitride (TaNx) thin films, where x indicates that TaNx is not generally stoechiometric, can be measured directly by XPS. This is the purpose of the present study. However, the XPS spectra of TaNx present electron energy loss spectroscopy (EELS) peaks that lead to a complex peak fitting, particularly for self-passivated thin films. A complete peak fitting procedure based upon Tougaard's background, the Doniach-Sunjic Function and EELS peaks, is presented. It is applied to two self-passivated TaNx thin films elaborated by reactive sputtering and presenting a different nitrogen content. The physical properties of these surfaces are interpreted in terms of Ta 4f7/2 chemical states directly dependent on the nitrogen content. The main results are discussed and improvements are proposed to the method. Copyright © 2008 John Wiley & Sons, Ltd.

Nanostructured multilayers constituted by alternate metallic (gold) and organic (alkyldithiol) layers, and grafted onto glass or silicon substrates are prepared and analysed. Such complex layers could be of interest as a new type of surfaces but also as localized dissipative zones particularly in the field of adhesion science. The formation and the structure of these model systems are examined using a number of techniques such as atomic force microscopy (AFM), wetting analysis (contact angles), X-ray photoelectron spectroscopy (XPS) and conductivity measurements. It is shown that, in terms of electrical conductivity, gold layers exhibit a percolation transition from an insulating granular structure to a conductive worm-like structure at a threshold thickness of about 5 nm. XPS (and wettability) analyses clearly indicate that the fractional coverage of the gold surface is about 30% with alkyldithiol and that these molecules are either grafted in a stand-up position or in the form of a loop. Moreover, a partial electrical connection between two successive gold layers is observed, confirming that the confined organic layer of alkyldithiol between them is too loosely organized to play the role of an insulating barrier. Copyright (C) 2007 John Wiley & Sons, Ltd.

The present study deals with the optimization of polyimide (PI) mechanical properties, obtained by Spark Plasma Sintering (SPS), by using a method combining Design of Experiments (DOE) with physical, structural, and mechanical characterizations. The effects of SPS parameters such as temperature, pressure, dwell time, and cooling rate on the density, mechanical properties, and structure of PI were investigated. The experimental results revealed that the mechanical properties of the material were optimized by raising the sintering temperature up to 350 degrees C. The optimized SPS processing parameters were a temperature of 350 degrees C, a pressure of 40 MPa, and a dwell time of 5 min. Under these conditions, a relative density of 99.6% was reached within only a few minutes. The corresponding mechanical properties consisted of Young's modulus of 3.43 GPa, a Shore D hardness of 87.3, and a compressive strength of 738 MPa for a maximum compressive strain of 61.8%. Moreover, when working at 320 degrees C and at 100 MPa, an increase in the dwell time was necessary to enhance the properties. Contrary to the other parameters, the cooling rate appeared to be a non-significant parameter. Finally, correlations between the PI structure and the mechanical properties were made to demonstrate the densification mechanisms. (c) 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41542.

This article presents two high-temperature thermoplastic powders which were sintered by spark plasma sintering in order to get homogeneous mechanical properties. Dense polyimide (PI) and polyetheretherketone (PEEK) specimens were obtained at temperatures as low as 320°C for PI and 200°C for PEEK, respectively. Relative densities higher than 99% were reached for both materials. In order to characterize their properties, in situ measurements with compression and hardness tests were carried out on sintered samples. This method allowed to obtain polymeric materials with improved mechanical properties. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40783.

This study investigates the adhesion, cytoskeletal changes, and resorptive activity of disaggregated rat osteoclasts cultured on polished slices of three biomaterials: crystalline synthetic hydroxyapatite (HA), carbonated hydroxyapatite (C-HA), and natural calcium carbonate (C). The surface chemistry of each substrate was defined by X-ray diffraction and IR spectroscopy, surface wettability by the dispersive, and the polar components of the surface energies. Osteoclast adhesion was modulated by the polar component of the surface energy: fewer (p < 0.01) osteoclasts adhered to C-HA (97 +/- 20/slice, surface energy 9 +/- 5 mJ/m2) than to HA (234 +/- 16/slice, surface energy 44 +/- 2 mJ/m2) or to C (268 +/- 37/slice, surface energy 58 +/- 0.5 mJ/m2). Actin rings, which are the cytoskeletal structure essential for resorption, developed on all three materials. The area of the actin ring, which is resorbed by local acidification, and the osteoclast area, which reflects osteoclast spreading, were both greater in osteoclasts cultured on HA and C-HA than in those cultured on C. C was resorbed, but HA and C-HA were not. Thus, the surface energy plays an essential role in osteoclast adhesion, whereas osteoclast spreading may depend on the surface chemistry, especially on protein adsorption and/or on newly formed apatite layers. Resorption may be limited to the solubility of the biomaterial.

Thermal characteristics of ethylene—vinylacetate (EVA) copolymers having vinylacetate contents ranging from 5 to 40 w/w % are studied by differential scanning calorimetry. It is first shown that EVA copolymers having a vinylacetate content lower than 30 w/w % obey the Flory and Burfield theories of copolymer crystallisation. The minimum sequence length of CH2 ethylenic entities required to participate in a crystalline lamella is also deduced. One can conclude that EVA copolymers represent cases of “total exclusion” of the noncrystallizable comonomer. Moreover, it is observed that when the vinylacetate content is increased, the relative quantity of polyethylene amorphous phase increases and the degree of crystallinity decreases; whereas the β transition temperature of a characteristic-oriented amorphous phase is kept constant. A phase model of ethylene-vinylacetate copolymers, based on an enrichment process of the interlamellar amorphous phase by polyethylene segments originating from the crystalline phase, at increasing vinylacetate content, is proposed. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 64: 1903–1912, 1997

The stress transfer from the matrix to the fibre in composite materials depends to a large extent on the level of adhesion between these materials. In the present study, the work of adhesion between carbon fibres and PEEK polymer is estimated from the surface characteristics of the fibre and the matrix and, more precisely, from the dispersive component of the surface energy and the acid–base character of both material, determined by inverse gas chromatography at infinite dilution. The interfacial shear strength at the carbon fibre/PEEK interface is measured also by means of a fragmentation test on the respective single-fibre composites. For PEEK polymer, it is shown that the acid–base characteristic of fibres and powder are different, indicating that the orientation of the macromolecules near the surface may be affected by the processing of such materials. Nevertheless, as already shown in previous studies for other systems, a linear relationship between the interfacial shear strength and the adhesion at the fibre/matrix interface can be established.