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The thermal resistance of carbon fiber–reinforced poly(phenylene sulfide) to harsh oxidative conditions is investigated through thermogravimetric experiments performed in an oxygen atmosphere. While these materials usually show great resistance against thermal decomposition in a nitrogen atmosphere, the experiments in oxygen reveal the total decomposition of both the matrix and the carbon fibers. The Gram–Schmidt signal, obtained by coupling thermogravimetric analysis in standard conditions with Fourier-transform infrared spectroscopy, exhibits multiple events, evidencing that the decomposition proceeds through distinct stages. The first step characterizes the char formation, while the second relates to its oxidative decomposition. A third step, only observed for composites, is interpreted as the signature of the oxidative decomposition of carbon fibers. To mimic the sudden elevation of temperature encountered during a fire, the analyses are performed at rates of up to 500 K min−1. These specific experimental conditions reveal a complex dependence of the thermogravimetric signature on the heating rate. Independent of the atmosphere, nitrogen or oxygen, the characteristic temperature of decomposition follows a bell-shape trend, resulting from the combination of lag effects and thermal-conductivity limitations. Additionally, the increase of the heating rate causes the Gram–Schmidt signal to evolve toward a broad peak with indistinct events. To investigate whether these changes affect the decomposition products, the infrared spectra, continuously recorded to probe the whole decomposition, are compared with those from the database. The char formation is characterized by the production of sulfur dioxide, while carbon dioxide is the main product emitted during both char and fiber oxidative decomposition. Owing to the merging of the decomposition stages, sulfur-dioxide detection is partly supplanted by that of carbon dioxide under fast elevations of temperature.

Dental surgery needs a biocompatible implant design that can ensure both osseointegration and soft tissue integration. This study aims to investigate the behavior of a hydroxyapatite-based coating, specifically designed to be deposited onto a zirconia substrate that was intentionally made porous through additive manufacturing for the purpose of reducing the cost of material. Layers were made via sol–gel dip coating by immersing the porous substrates into solutions of hydroxyapatite that were mixed with polyethyleneimine to improve the adhesion of hydroxyapatite to the substrate. The microstructure was determined by using X-ray diffraction, which showed the adhesion of hydroxyapatite; and atomic force microscopy was used to highlight the homogeneity of the coating repartition. Thermogravimetric analysis, differential scanning calorimetry, and Fourier transform infrared spectroscopy showed successful, selective removal of the polymer and a preserved hydroxyapatite coating. Finally, scanning electron microscopy pictures of the printed zirconia ceramics, which were obtained through the digital light processing additive manufacturing method, revealed that the mixed coating leads to a thicker, more uniform layer in comparison with a pure hydroxyapatite coating. Therefore, homogeneous coatings can be added to porous zirconia by combining polyethyleneimine with hydroxyapatite. This result has implications for improving global access to dental care.

Biodegradable PLA/PBSA multinanolayer nanocomposites were obtained from semi-crystalline poly(butylene succinate-co-butylene adipate) (PBSA) nanolayers filled with nanoclays and confined against amorphous poly(lactic acid) (PLA) nanolayers in a continuous manner by applying an innovative coextrusion technology. The cloisite 30B (C30B) filler incorporation in nanolayers was considered to be an improvement of barrier properties of the multilayer films additional to the confinement effect resulting to forced assembly during the multilayer coextrusion process. 2049-layer films of ~300 µm thick were processed containing loaded PBSA nanolayers of ~200 nm, which presented certain homogeneity and were mostly continuous for the 80/20 wt% PLA/PBSA composition. The nanocomposite PBSA films (monolayer) were also processed for comparison. The presence of exfoliated and intercalated clay structure and some aggregates were observed within the PBSA nanolayers depending on the C30B content. A greater reduction of macromolecular chain segment mobility was measured due to combined effects of confinement effect and clays constraints. The absence of both polymer and clays interdiffusions was highlighted since the PLA glass transition was unchanged. Besides, a larger increase in local chain rigidification was evidenced through RAF values due to geometrical constraints initiated by close nanoclay contact without changing the crystallinity of PBSA. Tortuosity effects into the filled PBSA layers adding to confinement effects induced by PLA layers have caused a significant improvement of water barrier properties through a reduction of water permeability, water vapor solubility and water vapor diffusivity. The obtaining barrier properties were successfully correlated to microstructure, thermal properties and mobility of PBSA amorphous phase.

Performing pyrolysis studies on polymer matrix composites, at rates that match the elevation of temperature met during a fire exposure, is of primary interest for the aeronautics field. In this study, one aspect of the material response under flame is investigated, which is the thermal degradation of the polymer matrix. Thermogravimetric analyses (TGA), up to five hundred Kelvins per minute, are performed on polyphenylene sulfide (PPS) and carbon fiber-reinforced polyphenylene sulfide (CF/PPS), to mimic the heating rate conditions commonly met during a fire. The influence of the heating rate regarding the PPS decomposition signature is discussed from both the residual mass and the characteristic temperature corresponding to the maximum rate of degradation. Then, the PPS thermal decomposition features are compared with those of several thermoplastic polymers and thermoplastic–based composites. It is observed that PPS stands out when subjected to fast elevation of temperature. Indeed, its amount of «char», obtained after thermal degradation, increases with the heating rate. To investigate possible mechanistic causes behind this singular behavior, the influence of the heating rate on the degradation mechanisms occurring into PPS and CF/PPS is investigated. TGA coupled with Fourier transform infrared spectroscopy (FTIR) is used to obtain the decomposition products. The results plaid for the coexistence of two main degradation mechanisms, being the random chain–scission and the depolymerization. Nevertheless, when the heating rate increases, the random chain–scission seemingly becomes the predominant mechanism along the whole process. Graphical abstract

In this paper, the calorimetric response of the amorphous phase was examined in hybrid nanocomposites which were prepared thanks to a facile synthetic route, by adding reduced graphene oxide (rGO), Cloisite 30B (C30B), or multiwalled carbon nanotubes (MWCNT) to lignin-filled poly(lactic acid) (PLA). The dispersion of both lignin and nanofillers was successful, according to a field-emission scanning-electron microscopy (FESEM) analysis. Lignin alone essentially acted as a crystallization retardant for PLA, and the nanocomposites shared this feature, except when MWCNT was used as nanofiller. All systems exhibiting a curtailed crystallization also showed better thermal stability than neat PLA, as assessed from thermogravimetric measurements. As a consequence of favorable interactions between the PLA matrix, lignin, and the nanofillers, homogeneous dispersion or exfoliation was assumed in amorphous samples from the increase of the cooperative rearranging region (CRR) size, being even more remarkable when increasing the lignin content. The amorphous nanocomposites showed a signature of successful filler inclusion, since no rigid amorphous fraction (RAF) was reported at the filler/matrix interface. Finally, the nanocomposites were crystallized up to their maximum extent from the glassy state in nonisothermal conditions. Despite similar degrees of crystallinity and RAF, significant variations in the CRR size were observed among samples, revealing different levels of mobility constraining in the amorphous phase, probably linked to a filler-dimension dependence of space filling.

The impact of the immersion in water on the morphology and the thermomechanical properties of a biocomposite made of a matrix of poly (lactic acid) (PLA) modified with an ethylene acrylate toughening agent, and reinforced with miscanthus fibers, has been investigated. Whereas no evidence of hydrolytic degradation has been found, the mechanical properties of the biocomposite have been weakened by the immersion. Scanning electron microscopy (SEM) pictures reveal that the water-induced degradation is mainly driven by the cracking of the fiber/matrix interface, suggesting that the cohesiveness is a preponderant factor to consider for the control of the biocomposite decomposition in aqueous environments. Interestingly, it is observed that the loss of mechanical properties is aggravated when the stereoregularity of PLA is the highest, and when increasing the degree of crystallinity. To investigate the influence of the annealing on the matrix behavior, crystallization at various temperatures has been performed on tensile bars of PLA made by additive manufacturing with an incomplete filling to enhance the contact area between water and polymer. While a clear fragilization occurs in the material crystallized at high temperature, PLA crystallized at low temperature better maintains its properties and even shows high elongation at break likely due to the low size of the spherulites in these annealing conditions. These results show that the tailoring of the mesoscale organization in biopolymers and biocomposites can help control their property evolution and possibly their degradation in water.

Fragility index and cooperativity length characterizing the molecular mobility in the amorphous phase are for the first time calculated in drawn polylactide (PLA). The microstructure of the samples is investigated from wide-angle X-ray scattering (WAXS) whereas the amorphous phase dynamics are revealed from broadband dielectric spectroscopy (BDS) and temperature-modulated differential scanning calorimetry (TMDSC). The drawing processes induce the decrease of both cooperativity and fragility with the orientation of the macromolecules. Post-drawing annealing reveals an unusual absence of correlation between the evolutions of cooperativity length and fragility. The cooperativity length remains the same compared to the drawn sample while a huge increase of the fragility index is recorded. By splitting the fragility index in a volume contribution and an energetic contribution, it is revealed that the amorphous phase in annealed samples exhibits a high energetic parameter, even exceeding the amorphous matrix value. It is assumed that the relaxation process is driven in such a way that the volume hindrance caused by the thermomechanical constraint is compensated by the acceleration of segmental motions linked to the increase of degrees of freedom. This result should also contribute to the understanding of the constraint slackening in the amorphous phase during annealing of drawn PLA, which causes among others the decrease of its barrier properties.

The present research aims at quantifying the impact of practicing a new coordination pattern with an online visual feedback on the postural coordination performed on a mechanical horse. Forty-four voluntary participants were recruited in this study. They were randomly assigned to four practice groups based on i) with or without feedback (i.e., group 1, control, did not receive the feedback; group 2, 3 and 4 received an online feedback during practice) and ii) the specific trunk/horse coordination to target during practice (group 1, target coordination = 180° (without feedback); group 2, target coordination = 0°; group 3, target coordination = 90°; group 4, target coordination = 180°). All participants performed pre-, practice, post- and retention sessions. The pre-, post- and retention sessions consisted of four trials, with one trial corresponding to one specific target coordination to maintain between their own oscillations and the horse oscillations (spontaneous, 0°, 90°, and 180°). The practice phase was composed of three different sessions during which participants received an online feedback about the coordination between their own oscillations and the horse oscillations. Results showed a significant change with practice in the trunk/horse coordination patterns which persisted even after one month (retention-test). However, all the groups did not show the same nature of change, evidenced by a high postural variability during post-test for 0° and 90° target coordination groups, in opposition to the 180° and spontaneous groups who showed a decrease in coordination variability for the 180° group. The coordination in anti-phase was characterized as spontaneously adopted by participants on the mechanical horse, explaining the ease of performing this coordination (compared to the 0° and 90° target coordination). The effect of online visual feedback appeared not only on the coordination pattern itself, but most importantly on its variability during practice, including concerning initially stable coordination patterns.

The present research aims at quantifying the impact of practicing a new coordination pattern with an online visual feedback on the postural coordination performed on a mechanical horse. Forty-four voluntary participants were recruited in this study. They were randomly assigned to four practice groups based on i) with or without feedback (i.e., group 1, control, did not receive the feedback; group 2, 3 and 4 received an online feedback during practice) and ii) the specific trunk/horse coordination to target during practice (group 1, target coordination = 180° (without feedback); group 2, target coordination = 0°; group 3, target coordination = 90°; group 4, target coordination = 180°). All participants performed pre-, practice, post- and retention sessions. The pre-, post- and retention sessions consisted of four trials, with one trial corresponding to one specific target coordination to maintain between their own oscillations and the horse oscillations (spontaneous, 0°, 90°, and 180°). The practice phase was composed of three different sessions during which participants received an online feedback about the coordination between their own oscillations and the horse oscillations. Results showed a significant change with practice in the trunk/horse coordination patterns which persisted even after one month (retention-test). However, all the groups did not show the same nature of change, evidenced by a high postural variability during post-test for 0° and 90° target coordination groups, in opposition to the 180° and spontaneous groups who showed a decrease in coordination variability for the 180° group. The coordination in anti-phase was characterized as spontaneously adopted by participants on the mechanical horse, explaining the ease of performing this coordination (compared to the 0° and 90° target coordination). The effect of online visual feedback appeared not only on the coordination pattern itself, but most importantly on its variability during practice, including concerning initially stable coordination patterns.