Production of nanofibrillated cellulose (CNF) has gained increasing attention during the last decades with its recent industrialization, but such a process consumes still too high of an amount of energy. Here, cellulose nanofibrils at high solid content (20−25 wt %) and consuming 60% less energy compared to conventional processes were produced from enzymatic and TEMPO-oxidized cellulose fibers thanks to a twin screw extruder equipped with kneading disks and fully flighted conveying screws. The morphology and properties of the produced CNF were characterized using optical microscopy, atomic force microscopy (AFM), mechanical properties, and light transmittance. CNF with a width in the range of 20−30 nm and mechanical properties close to those obtained with commercial CNF (Young's modulus around 15 GPa) were produced. However, results from the degree of polymerization and crystallinity showed that twin screw extrusion (TSE) degrades the fibers as far as the supermasscolloider grinder is concerned. TSE appears as a new mechanical treatment that allows producing CNF at high solid contents and with low energy demand, which is a real asset for nanocellulose industrialization.
The air permeability of a number of commercial fibrous carbon materials: soft non-woven felts, rigidized felts and rigid boards, based on either PAN-or Rayon-derived fibres presenting various diameters, graphitised or not, and consolidated by different methods, was measured and investigated. Consistent behaviours were found within families of closely related materials, but the diversity of porous structures prevented any model, including the very popular Tomadakis-Sotirchos equation, to fit all results. The Archie's coefficient and the tortuosity factor for viscous flow were thus calculated. Not only all data were perfectly aligned on one single master curve, but the analysis was extended to many other fibrous materials and the same master curve was found to be relevant. The Archie's coefficient thus appears to be an intrinsic property, purely defined by the material geometry, as it does not depend on the 1D, 2D or 3D-type of flow. A fitting equation was proposed, encompassing all fibrous materials in very broad ranges of porosities and porous structures.
The growing trend towards sustainable energy production, while intermittent, can meet all the criteria of energy demand through the use and development of high-performance thermal energy storage (TES). In this context, high-temperature hybrid TES systems, based upon the combination of fibrous carbon hosts and peritectic phase change materials (PCMs), are seen as promising solutions. One of the main conditions for the operational viability of hybrid TES is the chemical inertness between the components of the system. Thus, the chemical stability and compatibility of several commercial carbon felts (CFs) and molten lithium salts are discussed in the present study. Commercial CFs were characterised by elemental analysis, X-ray diffraction (XRD) and Raman spectroscopy before being tested in molten lithium salts: LiOH, LiBr, and the LiOH/LiBr peritectic mixture defined as our PCM of interest. The chemical stability was evaluated by gravimetry, gas adsorption and scanning electron microscopy (SEM). Among the studied CFs, the materials with the highest carbon purity and the most graphitic structure showed improved stability in contact with molten lithium salts, even under the most severe test conditions (750 °C). The application of the Arrhenius law allowed calculating the activation energy (in the range of 116 to 165 kJ mol−1), and estimating the potential stability of CFs at actual application temperatures. These results confirmed the applicability of CFs as porous hosts for stabilising peritectic PCMs based on molten lithium salts.
Carbon monoliths were tested as electrodes for vanadium redox batteries. The materials were synthesised by a hard-templating route, employing sucrose as carbon precursor and sodium chloride crystals as the hard template. For the preparation process, both sucrose and sodium chloride were ball-milled together and molten into a paste which was hot-pressed to achieve polycondensation of sucrose into a hard monolith. The resultant material was pyrolysed in nitrogen at 750 °C, and then washed to remove the salt by dissolving it in water. Once the porosity was opened, a second pyrolysis step at 900 °C was performed for the complete conversion of the materials into carbon. The products were next characterised in terms of textural properties and composition. Changes in porosity, obtained by varying the proportions of sucrose to sodium chloride in the initial mixture, were correlated with the electrochemical performances of the samples, and a good agreement between capacitive response and microporosity was indeed observed highlighted by an increase in the cyclic voltammetry curve area when the SBET increased. In contrast, the reversibility of vanadium redox reactions measured as a function of the difference between reduction and oxidation potentials was correlated with the accessibility of the active vanadium species to the carbon surface, i.e., was correlated with the macroporosity. The latter was a critical parameter for understanding the differences of energy and voltage efficiencies among the materials, those with larger macropore volumes having the higher efficiencies.
Vertically aligned carbon nanotubes (VACNT) are manufactured nanomaterials with excellent properties and great potential for numerous applications. Recently, research has intensified toward achieving VACNT synthesis on different planar and non-planar substrates of various natures, mainly dependent on the user-defined application. Indeed, VACNT growth has to be adjusted and optimized according to the substrate nature and shape to reach the requirements for the application envisaged. To date, different substrates have been decorated with VACNT, involving the use of diffusion barrier layers (DBLs) that are often insulating, such as SiO2 or Al2O3. These commonly used DBLs limit the conducting and other vital physico-chemical properties of the final nanomaterial composite. One interesting route to improve the contact resistance of VACNT on a substrate surface and the deficient composite properties is the development of semi-/conducting interlayers. The present review summarizes different methods and techniques for the deposition of suitable conducting interfaces and controlled growth of VACNT on diverse flat and 3-D fibrous substrates. Apart from exhibiting a catalytic efficiency, the DBL can generate a conducting and adhesive interface involving performance enhancements in VACNT composites. The abilities of different conducting interlayers are compared for VACNT growth and subsequent composite properties. A conducting interface is also emphasized for the synthesis of VACNT on carbonaceous substrates in order to produce cost-effective and high-performance nano-engineered carbon composites.
The synthesis of resorcinol-formaldehyde (RF) xerogels is versatile enough to provide materials with custom pore size distributions in the meso/macroporous range. Specifically, seven xerogels were synthesised by changing the pH of the same RF solution, from pH 3 to pH 6. The resulting materials presented meso/macropore size distributions with average pore sizes from <5 to 510 nm, as determined by Hg intrusion and N 2 adsorption. Most of the RF xerogels had very similar geometric densities, except for the gels obtained at the two highest pH values, which were more dense. Both flexural and uniaxial compression tests were carried out to determine the dependence of strength and stiffness on the porosity of the xerogels. The results followed a power-law relationship between the mechanical properties and the density of the materials. However, two series of RF xerogels were found to fit such law independently, with the gels obtained at the three most acidic pH values (pH 3-4) showing unexpectedly high compression moduli. Further characterisation of the xerogels microstructure revealed the existence of rod-like microstructures that would bear most loads during the compression tests. These microstructures would act as struts that, once broken, would cause the catastrophic failure (bursting) of the xerogel.
The ability of various commercial fibrous carbon materials to withstand stress and conduct heat has been evaluated through experimental and analytical studies. The combined effects of different micro/macro-structural characteristics were discussed and compared. Large differences in mechanical behavior were observed between the different groups or subgroups of fibrous materials, due to the different types of fibers and the mechanical and/or chemical bonds between them. The application of the Mooney–Rivlin model made it possible to determine the elastic modulus of soft felts, with a few exceptions, which were studied in-depth. The possible use of two different mechanical test methods allowed a comparison of the results in terms of elastic modulus obtained under different deformation regimes. The effective thermal conductivity of the same fibrous materials was also studied and found to be much lower than that of a single carbon fiber due to the high porosity, and varied with the bulk density and the fiber organization involving more or less thermal contact resistances. The thermal conductivity of most materials is highly anisotropic, with higher values in the direction of preferential fiber orientation. Finally, the combination of compression and transient thermal conductivity measurement techniques allowed the heat conduction properties of the commercial fibrous carbons to be investigated experimentally when compressed. It was observed that thermal conductivity is strongly affected under compression, especially perpendicular to the main fiber orientation.
A LiBr/LiOH non-eutectic mixture shows a potentially outstanding heat energy density of 800 J/g at a constant temperature, which makes it a very promising candidate for heat storage applications around 300 °C. However, salt-based phase change materials are known for their too low thermal conductivity which can question the thermal storage systems effective feasibility. The objective here is to infiltrate a carbon felt of high porosity (> 93%) with the LiBr/LiOH mixture to anticipate this deficiency. The device has to be adapted according to the properties and the characteristics of the studied storage and host materials. The developed procedure for the carbon felt infiltration with the synthesized binary system is presented. The optimised working conditions allow (1) minimizing the interaction time duration between the quartz tube and the salt-based mixture and, (2) verifying the good chemical compatibility of the mixture with the host matrix after infiltration.
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