scholarly journals Tuning the Morphological Properties of Cellulose Aerogels: An Investigation of Salt-Mediated Preparation

Author(s):  
Prakash Parajuli ◽  
Sanjit Acharya ◽  
Julia Shamshina ◽  
Noureddine Abidi

Abstract In this study, alkali and alkaline earth metal chlorides with different cationic radii (LiCl, NaCl, and KCl, MgCl2, and CaCl2) were used to gain insight into the behavior of cellulose solutions in the presence of salts. The specific focus of the study was evaluation of the effect of salts’ addition on the sol-gel transition of the cellulose solutions and on their ability to form monoliths, as well as evaluation of the morphology (e.g., specific surface area, pore characteristics, and microstructure) of aerocelluloses prepared from these solutions. The effect of the salt addition on the sol-gel transition of cellulose solutions was studied using rheology, and morphology of resultant aerogels was evaluated by Scanning Electron Microscopy (SEM) and Brunauer-Emmett-Teller (BET) analysis, while the salt influence on the aerocelluloses’ crystalline structure and thermal stability was evaluated using powder X-Ray Diffraction (pXRD) and Thermogravimetric Analysis (TGA), respectively. The study revealed that the effect of salts’ addition was dependent on the component ions and their concentration. The addition of salts in the amount below certain concentration limit significantly improved the ability of the cellulose solutions to form monoliths and reduced the sol-gel transition time. Salts of lower cationic radii had a greater effect on gelation. However, excessive amount of salts resulted in the formation of fragile monoliths or no formation of gels at all. Analysis of surface morphology demonstrated that the addition of salts resulted in a significant increase in porosity and specific surface area, with salts of lower cationic radii leading to aerogels with much larger (~1.5 and 1.6-fold for LiCl and MgCl2, respectively) specific surface area compared to aerocelluloses prepared with no added salt. Thus, by adding the appropriate salt into the cellulose solution prior to gelation, the properties of aerocelluloses that control material’s performance (specific surface area, density, and porosity) could be tailored for a specific application.

Cellulose ◽  
2021 ◽  
Author(s):  
Prakash Parajuli ◽  
Sanjit Acharya ◽  
Julia L. Shamshina ◽  
Noureddine Abidi

AbstractIn this study, alkali and alkaline earth metal chlorides with different cationic radii (LiCl, NaCl, and KCl, MgCl2, and CaCl2) were used to gain insight into the behavior of cellulose solutions in the presence of salts. The specific focus of the study was  on the evaluation of the effect of salts’ addition on the sol–gel transition of the cellulose solutions and on their ability to form monoliths, as well as the evaluation of the morphology (e.g., specific surface area, pore characteristics, and microstructure) of aerocelluloses prepared from these solutions. The effect of the salt addition on the sol–gel transition of cellulose solutions was studied using rheology, and morphology of resultant aerogels was evaluated by scanning electron microscopy and Brunauer–Emmett–Teller analysis, while the salt influence on the aerocelluloses’ crystalline structure and thermal stability was evaluated using powder X-ray diffraction and thermogravimetric analysis, respectively. The study revealed that the effect of salts’ addition was dependent on the component ions and their concentration. The addition of salts in the amount below certain concentration limit significantly improved the ability of the cellulose solutions to form monoliths and reduced the sol–gel transition time. Salts of lower cationic radii had a greater effect on gelation. However, excessive amount of salts resulted in the formation of fragile monoliths or no formation of gels at all. Analysis of surface morphology demonstrated that the addition of salts resulted in a significant increase in porosity and specific surface area, with salts of lower cationic radii leading to aerogels with much larger (~ 1.5 and 1.6-fold for LiCl and MgCl2, respectively) specific surface area compared to aerocelluloses prepared with no added salt. Thus, by adding the appropriate salt into the cellulose solution prior to gelation, the properties of aerocelluloses that control material’s performance (specific surface area, density, and porosity) could be tailored for a specific application. Graphic abstract


Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1340
Author(s):  
Jakub Marchewka ◽  
Piotr Jeleń ◽  
Izabela Rutkowska ◽  
Patryk Bezkosty ◽  
Maciej Sitarz

The aim of this work was to synthesize porous ceramic materials from the SiOC system by the sol-gel method and the subsequent pyrolysis. The usage of two types of precursors (siloxanes) was determined by Si/C ratio in starting materials. It allows us to control the size of the pores and specific surface area, which are crucial for the potential applications of the final product after thermal processing. Methyltrimethoxysilane and dimethyldiethoxysilane were mixed in three different molar ratios: 4:1, 2:1, and 1:1 to emphasize Si/C ratio impact on silicon oxycarbide glasses properties. Structure and microstructure were examined both for xerogels and obtained silicon oxycarbide materials. Brunauer-Emmett-Teller (BET) analysis was performed to confirm that obtained materials are porous and Si/C ratio in siloxanes precursors affects porosity and specific surface area. This kind of porous ceramics could be potentially applied as gas sensors in high temperatures, catalyst supports, filters, adsorbents, or advanced drug delivery systems.


2011 ◽  
Vol 10 (2) ◽  
pp. 25
Author(s):  
Anirut Leksomboon ◽  
Bunjerd Jongsomjit

In this present study, the spherical silica support was synthesized from tetraethyloxysilane (TEOS), water, sodium hydroxide, ethylene glycol and n-dodecyltrimethyl ammonium bromide (C12TMABr). The particle size was controlled by variation of the ethylene glycol co-solvent weight ratio of a sol-gel method preparation in the range of 0.10 to 0.50. In addition, the particle size apparently increases with high weight ratio of co-solvent, but the particle size distribution was broader. The standard deviation of particle diameter is large when the co-solvent weight ratio is more than 0.35 and less than 0.15. However, the specific surface area was similar for all weight ratios ranging from 1000 to 1300 m2/g. The synthesized silica was spherical and has high specific surface area. The cobalt was impregnated onto the obtained silica to produce the cobalt catalyst used for CO2 hydrogenation.</


Clay Minerals ◽  
2018 ◽  
Vol 53 (4) ◽  
pp. 665-674 ◽  
Author(s):  
Emmanuel Ajenifuja ◽  
Abimbola P.I. Popoola ◽  
Kabir O. Oyedotun ◽  
Olawale Popoola

ABSTRACTKaolin and diatomite are abundant and widely available geological materials that may immobilize or stabilize functional chemical species on their surfaces for various applications. Acid-treated kaolin and diatomite were intercalated with photocatalyst Ag-TiO2nanoparticles using the sol–gel technique to prepare nanocomposite ceramic materials. The nanocomposites were sintered between 900°C and 1000°C to induce thermal reactions and to enhance nanoparticle–substrate attachment. Chemical and thermal characterizations of the acid-treated materials and intercalated nanocomposites were performed with energy-dispersive X-ray (EDX) analysis and differential scanning calorimetry (DSC), respectively. The Brunauer–Emmett–Teller (BET)-specific surface area and scanning electron microscopy (SEM) were employed for physical and microstructural characterization of the nanocomposites, respectively. Morphological studies revealed a uniform distribution of Ag-TiO2nanocrystallites in pores and on mineral particle surfaces. The BET analysis showed remarkable surface and grain modification by sintering. Decreases in the BET-specific surface area were observed for the sintered ceramic nanocomposite, Ag-TiO2-kaolin (20.244 to 5.446 m2/g) and Ag-TiO2-diatomite (19.582 to 10.148 m2/g).


2013 ◽  
Vol 831 ◽  
pp. 263-266
Author(s):  
Chung Hsin Wu ◽  
Chao Yin Kuo ◽  
Chih Hao Lai ◽  
Wei Yang Chung

This study explored the decolorization of C.I. Reactive Red 2 (RR2) by the ultraviolet (UV)/TiO2, UV/TiO2 + In2O3, and UV/TiO2-In2O3 systems. The TiO2-In2O3 was generated by the sol-gel method and TiO2 + In2O3 was created by mixing TiO2 and In2O3 powders. The surface properties of TiO2, In2O3, and TiO2-In2O3 were analyzed by X-ray diffraction, a specific surface area analyzer, UV-vis spectroscopy, and scanning electron microscopy. The specific surface area of TiO2, In2O3, and TiO2-In2O3 was 29.5, 44.6, and 35.7 m2/g, respectively; additionally, the band gap of TiO2, In2O3, and TiO2-In2O3 was 2.95, 2.64, and 2.91 eV; respectively. The decolorization rate constant fit pseudo-first-order kinetics and that of the UV/TiO2, UV/TiO2 + In2O3, and UV/TiO2-In2O3 systems was 0.0023, 0.0031, and 0.0072 min-1; respectively.


2011 ◽  
Vol 403-408 ◽  
pp. 1205-1210
Author(s):  
Jaleh Babak ◽  
Ashrafi Ghazaleh ◽  
Gholami Nasim ◽  
Azizian Saeid ◽  
Golbedaghi Reza ◽  
...  

In this work ZnO nanocrystal powders have been synthesized by using Zinc acetate dehydrate as a precursor and sol-gel method. Then the products have been annealed at temperature of 200-1050°C, for 2 hours. The powders were characterized using X-ray diffraction (XRD), UV-vis absorption and photoluminescence (PL) spectroscopy. The morphology of refrence ZnO nanoparticles have been studied using Transmission Electron Microscope (TEM). During the annealing process, increase in nanocrystal size, defects and energy gap quantitative, and decrease in specific surface area have been observed.


2005 ◽  
Vol 23 (6) ◽  
pp. 497-508 ◽  
Author(s):  
Yu. Gnatyuk ◽  
N. Smirnova ◽  
A. Eremenko ◽  
V. Ilyin

Optically transparent, crack-free mesoporous titania and zirconia-doped titania thin films were fabricated by the sol—gel technique using the non-ionic amphiphilic triblock copolymer Pluronic P123 as the template. The structure and optical properties of these films were characterized using TEM, low-angle XRD, DTA/TG measurements, UV—vis spectroscopy and hexane adsorption investigations. It was found that addition of ZrO2 into the TiO2 matrix retarded sintering of the films, thereby increasing the specific surface area after treatment up to 500°C. The catalytic activity of the mesoporous TiO2 and TiO2/(5–30%) ZrO2 films in ethanol photo-oxidation increased with increasing specific surface area and surface acidity of the samples.


2013 ◽  
Vol 423-426 ◽  
pp. 523-527
Author(s):  
Xuan Liu ◽  
Zhen Fa Liu ◽  
Hao Lin Fu ◽  
Rui He ◽  
Li Hui Zhang

Phloroglucinol-resorcinol-formaldehyde organic aerogels (PRF) were prepared using phloroglucinol, resorcinol and formaldehyde in a sol-gel process, solvent replacement and drying at room temperature. The phloroglucinol-resorcinol-formaldehyde carbon aerogels (CPRF) were prepared by charring the PRF at high temperature under the aegis of helium flow. The microstructure of CPRF was characterized by infrared spectroscopy, specific surface area analyzer and scanning electron microscopy. The results showed that the CPRF had continuous network structure and high specific surface area.


2017 ◽  
Vol 19 (2) ◽  
pp. 56-60 ◽  
Author(s):  
Loghman Karimi

Abstract This study presents a facile approach for the preparation of MoS2 nanosheet decorated by porous titanium dioxide with effective photocatalytic activity. Mesoporous titanium dioxide nanostructures first synthesized by a hydrothermal process using titanium (III) chloride and then the MoS2/TiO2 were prepared through mixing of MoS2 nanosheet with mesoporous titanium dioxide under ultrasonic irradiation. The synthesized nanocomposite was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), and Brunauer-Emmett-Teller (BET) analysis. The results showed that the nanocomposite has mesoporous structure with specific surface area of 176.4 m2/g and pore diameter of 20 nm. The as-prepared MoS2/TiO2 nanocomposites exhibited outstanding photocatalytic activity for dye degradation under sunlight irradiation, which could be attributed to synergistic effect between the molybdenum disulfide nanosheet and mesoporous titanium dioxide. The photocatalytic performance achieved is about 2.2 times higher than that of mesoporous TiO2 alone. It is believed that the extended light absorption ability and the large specific surface area of the 2D MoS2 nanosheets in the nanocomposite, leading to the enhanced photocatalytic degradation activity.


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