Microwave drying as an effective method to obtain porous carbon xerogels; ; et al in Journal of Non-Crystalline Solids (2008), 354(33), 4024-4026 Microwave drying was used to prepare resorcinol-formaldehyde aqueous gels, without performing any pretreatment, and to see whether it was possible to use this drying option to obtain porous carbon ... [more ▼] Microwave drying was used to prepare resorcinol-formaldehyde aqueous gels, without performing any pretreatment, and to see whether it was possible to use this drying option to obtain porous carbon xerogels with controlled textural properties. By using microwave drying, the process for obtaining carbon gels is greatly simplified, textural properties are controlled likewise with other drying methods, but the time involved in the process is significantly reduced and no pretreatment is necessary. Therefore, microwave drying could help to simplify the carbon xerogels synthesis and reduce the associated costs. (C) 2008 Elsevier B.V. All rights reserved. [less ▲] Detailed reference viewed: 25 (2 ULg) Tailoring the textural properties of activated carbon xerogels by chemical activation with KOH; ; Pirard, Jean-Paul et alin Microporous & Mesoporous Materials (2008), 115(3), 480-490 Resorcinol-formaldehyde xerogels synthesised with different resorcinol/sodium carbonate molar ratios were chemically activated either after drying or after drying and pyrolysis, using potassium hydroxide ... [more ▼] Resorcinol-formaldehyde xerogels synthesised with different resorcinol/sodium carbonate molar ratios were chemically activated either after drying or after drying and pyrolysis, using potassium hydroxide. It was found that organic (i.e. dried) and carbon (i.e. pyrolysed) xerogels behave differently when subjected to chemical activation. In the case of carbon xerogels, the increase in the microporosity takes place without any significant modification to the meso/macroporosity formed during the synthesis step, leading to micromesoporous or micro-macroporous materials with a larger micropore volume. Furthermore, control of the microporosity is possible because its development depends on the amount of KOH used. However, when organic xerogels are activated, mainly microporous materials with BET specific surface areas of up to 2000 m(2) g(-1) are obtained, there hardly remaining any of the meso/macroporosity formed during the gel synthesis. Thus, the combination of different synthesis conditions and chemical activation with potassium hydroxide allows the textural properties of carbon xerogels to be tailored at both micropore and meso/macropore levels. (c) 2008 Elsevier Inc. All rights reserved. [less ▲] Detailed reference viewed: 21 (1 ULg) Critical opalescence points to thermodynamic instability:relevance to small-angle X-ray scattering of resorcinol–formaldehyde gel formation at low pHGommes, Cédric ; Job, Nathalie ; Pirard, Jean-Paul et alin Journal of Applied Crystallography (2008), 41(4), 663-668 During the formation at low pH of resorcinol–formaldehyde gels with a structure in the micrometre range, small-angle X-ray scattering exhibits a nonmonotonic intensity variation as a function of reaction ... [more ▼] During the formation at low pH of resorcinol–formaldehyde gels with a structure in the micrometre range, small-angle X-ray scattering exhibits a nonmonotonic intensity variation as a function of reaction time. The data are analyzed in terms of scattering by statistical fluctuations of polymer concentration, the amplitude of which is maximal close to the critical point for phase separation between polymer and solvent. The data do not carry any morphological information, but they unambiguously show that the driving force of the gel formation is a thermodynamic instability of the polymerizing solution. [less ▲] Detailed reference viewed: 64 (15 ULg) Carbon xerogels as catalyst supportsJob, Nathalie ; Léonard, Angélique ; Lambert, Stéphanie et alPoster (2007, August) Detailed reference viewed: 18 (4 ULg) Water desorption isotherms of resorcinol-formaldehyde and carbon xerogelsLéonard, Angélique ; ; Job, Nathalie et alPoster (2007, July 15) Detailed reference viewed: 5 (3 ULg) Water desorption isotherms of resorcinol-formaldehyde and carbon xerogelsLéonard, Angélique ; ; Job, Nathalie et alin The American Carbon Society (Ed.) Proceedings of Carbon 2007 (2007, July) Detailed reference viewed: 28 (4 ULg) Xérogels de carbone comme supports de catalyseurs pour cathodes de piles à combustibles PEMJob, Nathalie ; Marien, José ; Lambert, Stéphanie et alConference (2007, March 19) Detailed reference viewed: 4 (1 ULg) Rheological determination of the sol-gel transition during the aqueous synthesis of resorcinol-formaldehyde resinsJob, Nathalie ; ; Crine, Michel et alin Colloids and Surfaces A : Physicochemical and Engineering Aspects (2007), 293(1-3), 224-228 The sol-gel transition of organic gels prepared by polycondensation of resorcinol (R) with formaldehyde (F) in presence of sodium carbonate (C) was monitored by small amplitude oscillatory measurements ... [more ▼] The sol-gel transition of organic gels prepared by polycondensation of resorcinol (R) with formaldehyde (F) in presence of sodium carbonate (C) was monitored by small amplitude oscillatory measurements, at a single frequency. The gelation time (t(g)) was determined from the evolution of the storage (G) and loss (G") moduli versus time. The influence of two synthesis variables, the resorcinol/sodium carbonate ratio (R/C) and the synthesis temperature (7), was investigated. The gelation time was found to decrease with increasing synthesis temperature and decreasing R/C ratio. The apparent activation energy of the reactional system leading to the gelation, calculated from the gelation times obtained between 50 and 90 degrees C, was found to be close to 80 kJ mol(-1) and independent of the R/C ratio. (c) 2006 Elsevier B.V. All rights reserved. [less ▲] Detailed reference viewed: 96 (11 ULg) Compressing some sol-gel materials reduces their stiffness: a textural analysisGommes, Cédric ; Job, Nathalie ; Blacher, Silvia et alin Studies in Surface Science and Catalysis (2007), 160 The mechanical behaviour of two series of silica and of resorcinol xerogels is analyzed by mercury porosimetry. The data are expressed as pressure-density curves, which enables textural information to be ... [more ▼] The mechanical behaviour of two series of silica and of resorcinol xerogels is analyzed by mercury porosimetry. The data are expressed as pressure-density curves, which enables textural information to be obtained. In particular, it is shown that some of the analyzed samples exhibit a marked lowering of their mechanical stiffness upon compression. This observation is analyzed in terms of the collapse of the sample’s porosity and of the heterogeneity of the microstructure. [less ▲] Detailed reference viewed: 21 (4 ULg) Synthesis of transition metal-doped carbon xerogels by cogelationJob, Nathalie ; Pirard, René ; Vertruyen, Bénédicte et alin Journal of Non-Crystalline Solids (2007), 353(24-25), 2333-2345 The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is ... [more ▼] The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is to anchor the metal to the polymer so that the former does not sinter during the pyrolysis step leading to porous carbon. Cu-, Ni-, Pd- or Pt-loaded gels were prepared by this technique. After drying and pyrolysis, Pd and Pt were obtained as metal nanoparticles (2-5 nm in diameter) inserted in the carbon nodules, when the complexing agent and the synthesis conditions were well chosen. These small metal particles were inaccessible to reactive gases, probably due to carbon deposit at the metal surface during pyrolysis: CO almost did not chemisorb. Oxidation of the support or pyrolysis under reductive atmosphere was applied to the metal-doped gels and carbons in order to make the surface of the metal particles accessible, but these treatments develop the macropores only. The cogelation process is then suitable to prepare metal nanoparticles protected from the outside by encapsulation in the carbon matrix. (C) 2007 Elsevier B.V. All rights reserved. [less ▲] Detailed reference viewed: 72 (22 ULg) Sol-gel synthesis of supported metalsHeinrichs, Benoît ; Lambert, Stéphanie ; Job, Nathalie et alin Regalbuto, John R. (Ed.) Catalyst Preparation : Science and Engineering (2007) Detailed reference viewed: 24 (14 ULg) Carbon xerogels as catalyst supports for PEM fuel cell cathodeJob, Nathalie ; ; Lambert, Stéphanie et alConference (2007) Detailed reference viewed: 14 (1 ULg) Towards the production of carbon xerogel monoliths by optimizing convective drying conditionsJob, Nathalie ; ; Pirard, Jean-Paul et alin Carbon (2006), 44(12), 2534-2542 Resorcinol-formaldehyde hydrogels prepared at various resorcinol/sodium carbonate ratios, R/C, were convectively air dried. The influence of the drying operating conditions, i.e. air temperature and ... [more ▼] Resorcinol-formaldehyde hydrogels prepared at various resorcinol/sodium carbonate ratios, R/C, were convectively air dried. The influence of the drying operating conditions, i.e. air temperature and velocity, on the pore texture, shrinkage and cracking of the dried gels were investigated. Shrinkage was found to be isotropic. The shrinkage behaviour and the textural properties of the gels are independent of the drying operating conditions, but are completely determined by the value of the synthesis variables. The analysis of the drying kinetics shows two main drying periods. During the first phase, shrinkage occurs and the external surface of the material remains completely wet: heat and mass transfers are limited by external resistances located in a boundary layer. When shrinkage stops, the second period begins: the evaporation front recedes inside the solid and internal transfer limitations prevail. The drying time can be reduced by increasing the air temperature and/or velocity, but the temperature increase is limited when monolithicity is required, especially when the pores are small. For example, at a temperature of 160 degrees C and a velocity of 2 m/s, about 1 h is needed to dry a 2.8 cm in diameter and 1 cm in height cylinder containing macropores (pore width > 50 nm after drying). The same cylinder presenting small mesopores (pore width = 10-15 nm after drying) requires 20 h at 30 degrees C and 2 m/s to reach complete dryness without the development of cracks. (c) 2006 Elsevier Ltd. All rights reserved. [less ▲] Detailed reference viewed: 57 (8 ULg) Study of shrinkage and cracks development during the production of resorcinol-formaldehyde xerogels by µ-CTLéonard, Angélique ; ; Job, Nathalie et alPoster (2006, September 25) Detailed reference viewed: 8 (0 ULg) Time-resolved SAXS study of the formation of resorcinol-formaldehyde aqueous gelsJob, Nathalie ; Gommes, Cédric ; et alPoster (2006, August 06) Detailed reference viewed: 14 (0 ULg) Cu/Carbon xerogel catalysts for the selective catalytic reduction of NO by NH3 : effect of the pore texture; Job, Nathalie ; Pirard, Jean-Paul et alPoster (2006, July 12) Detailed reference viewed: 1 (0 ULg) Encapsulation of transition metal nanoparticles in carbon xerogels by cogelationJob, Nathalie ; Pirard, René ; Marien, José et alPoster (2006, June 08) Detailed reference viewed: 4 (0 ULg) Elimination des limitations de transfert de matière en catalyse supportée sur carbone par utilisation de supports de type xérogel de carboneJob, Nathalie ; Heinrichs, Benoît ; Léonard, Angélique et alConference (2006, April 03) Detailed reference viewed: 2 (0 ULg) Synthesis optimization of organic xerogels produced from convective air-drying of resorcinol-formaldehyde gelsJob, Nathalie ; ; Marien, José et alin Journal of Non-Crystalline Solids (2006), 352(1), 24-34 Resorcinol-formaldehyde gels were produced at 50, 70 and 90 degrees C and with three different R/C ratios (500, 1000 and 2000). The effect of these variables combined with that of aging time was studied ... [more ▼] Resorcinol-formaldehyde gels were produced at 50, 70 and 90 degrees C and with three different R/C ratios (500, 1000 and 2000). The effect of these variables combined with that of aging time was studied in order to optimize the synthesis conditions. The convective air-drying process was used, and the drying duration was studied with regard to the synthesis conditions. The aging time has no effect on the pore texture after 24 h at 90 degrees C or 48 h at 70 C, whatever the R/C value. The synthesis-aging step can be shortened by increasing the temperature. Nevertheless, the pore size tends then to decrease, especially when R/C is high, but this can be counterbalanced by increasing R/C. Moreover, bubbles often appear in the gel at high synthesis temperature, which limits the temperature to about 70 degrees C in the case of monolithic parts. At 70 degrees C and with an air velocity of 2 m/s, the elimination of 90% of the solvent requires 1 h drying when the pore size reaches 400-600 nm, 2.5 h for 50 nm wide pores and 3 h when the pore size decreases to 15-20 nm. The drying duration does not exceed 8 h in all cases and could be shortened by increasing the temperature at the end of the process. (c) 2005 Elsevier B.V. All rights reserved. [less ▲] Detailed reference viewed: 30 (1 ULg) Matériaux carbonés poreux de texture contrôlée préparés par procédé sol-gel et leur utilisation en catalyse hétérogèneJob, Nathalie ![]() Doctoral thesis (2006) Detailed reference viewed: 5 (0 ULg) |
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