Centre de Mise en Forme des Matériaux

Anodization of titanium and its alloys is an important surface treatment, especially for adhesion applications, but is not as well studied as for aluminium alloys. This paper deals with the morphological, structural and physicochemical characterization of anodic oxide films grown on titanium and Ti–6Al–4V (TA6V) in chromic acid solution without (CA) or with (CA/HF) hydrofluoric acid addition. Several investigations methods are used: high-resolution scanning electron microscopy (HR-SEM), reflection high-energy electron diffraction (RHEED), x-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS), nuclear reaction analysis (NRA) and wetting angle measurements. The occurrence and morphology of the nanoporous structure for CA/HF anodization are described. The compact films grown in CA solution are amorphous and the porous films grown in the CA/HF solution are partially crystalline. The thickness and morphology of the films are described and discussed as a function of the anodizing conditions and of the composition of the underlying substrate. The composition of the film appears to be TiO2+Al2O3 (with Ti/Al atomic ratio ∽5), with incorporation of fluorine from the solution in the porous films and of small quantities of vanadium in the films that are grown. The specific role played by the Cr(VI) and F species on the film growth-and-dissolution formation process is discussed and a growth mechanism is proposed. Copyright © 1999 John Wiley & Sons, Ltd.

We present the first application of an artificial neural network trained through a deep reinforcement learning agent to perform active flow control. It is shown that, in a two-dimensional simulation of the Kármán vortex street at moderate Reynolds number ( $Re=100$ ), our artificial neural network is able to learn an active control strategy from experimenting with the mass flow rates of two jets on the sides of a cylinder. By interacting with the unsteady wake, the artificial neural network successfully stabilizes the vortex alley and reduces drag by approximately 8 %. This is performed while using small mass flow rates for the actuation, of the order of 0.5 % of the mass flow rate intersecting the cylinder cross-section once a new pseudo-periodic shedding regime is found. This opens the way to a new class of methods for performing active flow control.

New highly porous pure cellulose aerogel-like material called "aerocellulose" was prepared from aqueous cellulose/NaOH solutions. Solutions were gelled to obtain shaped three-dimensional objects, then cellulose was regenerated and dried in supercritical conditions using CO2. The porosity of aerocellulose is higher than 95% with pore sizes distribution from a few tens of nanometers to a few tens of micrometers. The internal specific surface area is around 200-300 m2/g, and density ranges from 0.06 to 0.3 g/cm3, depending on the preparation conditions. The influence of cellulose DP and concentration, of the addition of a surfactant leading to solution foaming, of gelation conditions and the temperature and acidity of regenerating bath on the morphology of aerocellulose has been studied. The results are compared with another type of aerocellulose that was prepared from cellulose/NMMO solutions.

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Steady state shear flow of different types of cellulose (microcrystalline, spruce sulfite and bacterial) dissolved in 1-ethyl-3-methylimidazolium acetate was studied in a large range of concentrations (0-15%) and temperatures (0-100 degrees C). Newtonian flow was recorded for all experimental conditions; these viscosity values were used for detailed viscosity-concentration and viscosity-temperature analysis. The exponent in the viscosity-concentration power law was found to be around 4 for temperatures from 0 to 40 degrees C, which is comparable with cellulose dissolved in other solvents, and around 2.5-3 for 60-100 degrees C. Intrinsic viscosities of all celluloses decreased with temperature, indicating a drop in solvent thermodynamic quality with heating. The data obtained can be reduced to a master plot of viscosity versus (concentration x intrinsic viscosity) for all celluloses studied in the whole temperature range. Mark-Houwink exponents were determined: they were lower than that for cellulose dissolved in LiCl/N,N-dimethylacetamide at 30 degrees C and close to theta-value. Viscosity-inverse temperature plots showed a concave shape that is dictated by solvent temperature dependence. The values of the activation energies calculated within Arrhenius approximation are in-line with those obtained for cellulose of comparable molecular weights in other solvents.

A detailed study of the production of polysaccharide aerogel (bio-aerogel) particles from lab to pilot scale is surveyed in this article. An introduction to various droplets techniques available in the market is given and compared with the lab scale production of droplets using pipettes and syringes. An overview of the mechanisms of gelation of polysaccharide solutions together with non-solvent induced phase separation option is then discussed in the view of making wet particles. The main steps of particle recovery and solvent exchange are briefly described in order to pass through the final drying process. Various drying processes are overviewed and the importance of supercritical drying is highlighted. In addition, we present the characterization techniques to analyse the morphology and properties of the aerogels. The case studies of bio-aerogel (agar, alginate, cellulose, chitin, κ-carrageenan, pectin and starch) particles are reviewed. Potential applications of polysaccharide aerogel particles are briefly given. Finally, the conclusions summarize the prospects of the potential scale-up methods for producing bio-aerogel particles.

Johnson-Cook constitutive model is still the most used model in metal cutting simulation, although several drawbacks reported in the literature. A high number of Johnson-Cook model parameters can be found in the literature for the same work material. One question that may arise is “What is the most suitable set of Johnson-Cook model parameters for a given material?”. The present paper puts in evidence some issues related with the selection of these parameters from the literature. In this contribution, two sets of Johnson-Cook model parameters for Ti-6A-4 V are evaluated, using three types of metal cutting models. These models are based on three different formulations: Lagrangian, Arbitrary Eulerian-Lagrangian (ALE) and Couple Lagrangian-Eulerian (CEL). This evaluation is based on the comparison between measured and predicted chip geometry, chip compression ratio, forces, plastic deformation and temperature distributions.

Monolithic pectin aerogels, aeropectins, were prepared via dissolution-gelation-coagulation and subsequent drying with supercritical CO2. Aeropectin had pore sizes that varied from mesopores to small macropores and compression moduli in the range from 4 to 18 MPa. Aeropectins show plastic deformation up to 60% strain before the pore walls collapse. Pectin aerogels have a thermal conductivity below that of air in ambient conditions, making them new thermal superinsulating fully biomass-based materials. The contribution of gas and solid conduction plus radiative heat transfer were determined and discussed.

The aim of this work is to present a quantitative analysis of features involved in recovery during annealing of deformed Tantalum.In pure metals where crystalline defects usually have high mobility, dislocation annihilation and rearrangement occur to a great extent prior to recrystallization.Therefore a complete understanding of recrystallization cannot be accomplished without an advanced knowledge of the recovery phenomenon.Depending on whether dislocations induce a measurable curvature in the crystal lattice or not, they are called Geometrically Necessary Dislocations (GNDs) or Statistically Stored Dislocations (SSDs) respectively.In the present work only GNDs are considered.For this purpose electron backscatter diffraction (EBSD) is an advantageous technique to obtain statistically representative results when compared to Transmission Electron Microscopy (TEM).However, a quantitative analysis of GNDs from EBSD data is not straightforward.Since local misorientations are induced by the curvature of the crystal lattice caused by GNDs, GNDs analysis can be done using local misorientations.However the values obtained from this analysis are step size dependent and influenced by the measurement noise.Reasoning on the basis that when the step size tends to zero, local misorientation should also tend to zero, measurement noise can be estimated [1].The measurement noise appears to notably be very much dependent on the amplitude of local misorientations, which must be considered in the perspective of GND density calculation.

Abstract A global computation model for self‐wiping corotating twin screw extruders is proposed. Based on a ID approximated approach, it has been validated by comparison with experimentation and more sophisticated numerical models. It allows one to obtain, for any screw profile including left‐and right‐handed screw elements and kneading discs, the profile along the screws of the main flow variables, such as pressure, mean temperature, residence time, and filling ratio. Owing to the approximations made, this model can be easily and rapidly run on a personal computer or a workstation. Important applications may be found in screw profile design, scaleup, compounding or reactive extrusion.

Abstract Rate form constitutive equations of elasto‐viscoplastic type are expressed in a manner similar to that of classical metals, but the viscoplastic part, which is no longer incompressible, is related to the rate of variation of porosity. An incremental and implicit algorithm has been implemented in a finite element program in order to simulate hot isostatic pressing of an Astroloy powder. Temperature distributions are shown to induce strong density variations in real parts during hot isostatic pressing (HIP). For one particular turbine disk, we tested the sensitivity of the final shape to different processing parameters. Computed final shapes compare well with experimental ones.

The rheology of rigid rod cellulose whisker suspensions has been investigated. The isotropic-at-rest suspension flow curves show two plateaus, one at low shear rates and another at high shear rates, that reflect the flow of isotropic (at low shear rates) or oriented (at high shear rates) suspensions. From the low shear rate viscosity plateau vs concentration, we see that the system is in the semidilute region above 0.02 wt %, in agreement with the theoretical predictions. From the same curve, we can estimate a maximum packing concentration of whiskers rods that corresponds to the experimentally measured isotropic-to-anisotropic transition. The high shear rate plateau viscosity data show that the suspension is still in the dilute state above 0.6 wt %. The critical concentration at the dilute−semidilute transition is thus strongly dependent on the state of order, which suggests that care has to be taken when measuring parameters extracted from flowing solutions or suspensions, as for example occurring with Ubbelhode viscometry. Above a certain critical concentration, the suspensions become anisotropic at rest. The viscosity vs concentration curve has a maximum that vanishes at high shear rates as for liquid crystalline polymer solutions. Rheological and rheo-optical observations show fast inception and relaxation of both the rheological functions and the texture, in complete contrast with liquid crystalline polymer solutions.

ABSTRACT Gluten‐glycerol dough was extruded under a variety of processing conditions using a corotating self‐wiping twin‐screw extruder. Influence of feed rate, screw speed, and barrel temperature on processing parameters (die pressure, product temperature, residence time, specific energy) were examined. Use of flow modeling was successful for describing the evolution of the main flow parameters during processing. Rheological properties of extruded samples exhibited network‐like behavior and were characterized and modeled by Cole‐Cole distributions. Changes in molecular sizes of proteins during extrusion were measured by chromatography and appeared to be correlated to molecular size between network strands, as derived from the rheological properties of the materials obtained. Depending on operating conditions, extrudates presented very different surface aspects, ranging from very smooth‐surfaced extrudates with high swell to completely broken extrudates. The results indicated that extrudate breakup was caused by increasing network density, and some gliadins may have acted as cross‐linking agents. Increasing network density resulted in decreasing mobility of polymeric chains, and “protein melt” may no longer have been able to support the strain experienced during extrusion through the die. Increasing network density was reflected in increased plateau modulus and molecular size of protein aggregates. Increasing network structure appeared to be induced by the severity of the thermomechanical treatment, as indicated by specific mechanical energy input and maximum temperature reached.

Abstract The equations for steady isothermal spinning of a viscoelastic liquid are solved for a fluid model with constant modulus and a single constant relaxation time. High stress levels are predicted for elastic liquids, and the velocity approaches a linear profile in the limit of maximum drawdown. These predictions are in accordance with the observed behavior of polymeric liquids in isothermal spinning. Relaxation times computed from spinning data of Spearot and Metzner and Acierno et al. for four low density polyethylene melts are comparable to those measured rheogoniometrically, though the spinning relaxation times are 20 to 80% larger.

The viscosities of microcrystalline cellulose dissolved in 1-ethyl-3-methylimidazolium acetate (EMIMAc) and in 1-butyl-3-methylimidazolium chloride (BMIMCl) were studied in detail as a function of polymer concentration and temperature. The goal was to compare the flow of solutions, macromolecule hydrodynamic properties in each solvent, and the activation energies of viscous flow. Intrinsic viscosities were determined using the truncated form of the general Huggins equation. In both solvents cellulose intrinsic viscosity decreases with increasing temperature, indicating the decrease of solvent thermodynamic quality. The activation energies for both types of cellulose solutions were calculated. For cellulose-EMIMAc the Arrhenius plot showed a concave shape, and thus the Vogel-Tamman-Fulcher (VTF) approach was used. We suggest an improved method of data analysis for the determination of VTF constants and demonstrate that cellulose-EMIMAc solution viscosity obeys VTF formalism. Once the dependences of Arrhenius activation energy and VTF pseudo-activation energy were obtained for the whole range of concentrations studied, they were all shown to be described by a simple power-law function of polymer concentration.

Aerogels are a special class of nanostructured materials with very high porosity and tunable physicochemical properties. Although a few types of aerogels have already reached the market in construction materials, textiles and aerospace engineering, the full potential of aerogels is still to be assessed for other technology sectors. Based on current efforts to address the material supply chain by a circular economy approach and longevity as well as quality of life with biotechnological methods, environmental and life science applications are two emerging market opportunities where the use of aerogels needs to be further explored and evaluated in a multidisciplinary approach. In this opinion paper, the relevance of the topic is put into context and the corresponding current research efforts on aerogel technology are outlined. Furthermore, key challenges to be solved in order to create materials by design, reproducible process technology and society-centered solutions specifically for the two abovementioned technology sectors are analyzed. Overall, advances in aerogel technology can yield innovative and integrated solutions for environmental and life sciences which in turn can help improve both the welfare of population and to move towards cleaner and smarter supply chain solutions.

Starch aerogels were prepared via dissolution in water (thermomechanical treatment), retrogradation, solvent exchange, and drying with supercritical CO 2 . Amylose content in starches was varied from 0 to 100%. The aerogels’ bulk density, morphology, specific surface area, thermal conductivity, and mechanical properties under compression were investigated. Pea starch aerogels had one of the highest specific surface area and lowest density and thermal conductivity (0.021–0.023 W/m·K), with the latter indicating that a new thermal superinsulation material was obtained. A detailed study of the influence of processing parameters on pea starch aerogels properties showed the importance of retrogradation time which decreases specific surface area and increases mechanical properties and thermal conductivity. Finally, a comparison of starch aerogel thermal conductivity with that of other bioaerogels is performed.

Abstract This paper presents a mathematical and numerical model developed for coupling the various physical phenomena (electromagnetic, thermal and mechanical) taking place in axisymmetrical induction heating processes. All three electromagnetic, thermal and mechanical models are time dependent and take full account of the electromagnetic and thermal non‐linear effect especially with magnetic materials. The electromagnetic problem is discretized and solved in the workpiece, air and inductors. The heat transfer equation and the mechanical equilibrium equations are solved in the workpiece only, both using a finite element method. The mechanical model can take into account thermoelastic–plastic behaviour for the part. The model has been successfully applied to several cases of induction heating. Comparisons between numerical and experimental results show an excellent agreement. Copyright © 2003 John Wiley & Sons, Ltd.

Abstract Summary: Five modes describing the behaviour of cellulose fibres dipped in a chemical have been identified: Mode 1: Fast dissolution by disintegration into fragments Mode 2: Large swelling by ballooning, and dissolution Mode 3: Large swelling by ballooning, and no dissolution Mode 4: Homogeneous swelling, and no dissolution Mode 5: No swelling and no dissolution In the case of the behaviour of wood and cotton cellulose fibres in N‐methylmorpholine‐N‐oxide (NMMO) and water mixtures, four domains of water content have been identified. Below 17% of water up to monohydrate (13%), the fibres are disintegrated into rod‐like fragments and dissolve (mode 1). In NMMO – water mixtures containing 19–24% water, the cellulose fibres exhibit a heterogeneous swelling by forming balloons (composed of dissolved cellulose holds inside a membrane) separated with non‐swollen sections. The whole fibre will completely dissolve (mode 2) in four successive steps (growth of the balloons, burst of the balloons, dissolution of the non‐swollen sections and finally dissolution of the membrane). With still greater water contents (25–30%), only the ballooning phenomenon is observed, with a partial dissolution inside the balloon (mode 3). Above 35% of water, the fibres swell homogeneously and are not dissolving (mode 4).

Silica aerogels are excellent thermal insulators, but their brittle nature has prevented widespread application. To overcome these mechanical limitations, silica-biopolymer hybrids are a promising alternative. A one-pot process to monolithic, superinsulating pectin-silica hybrid aerogels is presented. Their structural and physical properties can be tuned by adjusting the gelation pH and pectin concentration. Hybrid aerogels made at pH 1.5 exhibit minimal dust release and vastly improved mechanical properties while remaining excellent thermal insulators. The change in the mechanical properties is directly linked to the observed "neck-free" nanoscale network structure with thicker struts. Such a design is superior to "neck-limited", classical inorganic aerogels. This new class of materials opens up new perspectives for novel silica-biopolymer nanocomposite aerogels.