scholarly journals Tuning the morphological properties of cellulose aerogels: an investigation of salt-mediated preparation

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

2021 ◽  
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.


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.</


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.


NANO ◽  
2018 ◽  
Vol 13 (04) ◽  
pp. 1850036 ◽  
Author(s):  
Guiqiang Diao ◽  
Hao Li ◽  
Hao Liang ◽  
Iryna Ivanenko ◽  
Tetiana Dontsova ◽  
...  

Multi-walled carbon nanotubes (MWCNTs) were synthesized onto a series of individual and bimetallic catalysts by the chemical vapor deposition (CVD) of acetylene at low temperature (600[Formula: see text]C). The catalysts were prepared by two methods, i.e., precipitation and sol–gel, with two different carriers – MgO and Al2O3. The catalysts were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermal gravimetric (TG) analysis, low-temperature adsorption of nitrogen. The yield of the MWCNTs was calculated in two ways, while the highest yield of 800% was achieved onto the two-component NiO/Co2O3/MgO catalyst, SEM and transmission electron microscopy (TEM) results confirm that uniform tube-like structure MWCNTs with the yield of 410% were obtained onto Co2O3/Al2O3 catalyst. These MWCNTs are smooth and pointing in the same direction. Their tube diameter is about 20[Formula: see text]nm, which is the smallest around all observed MWCNTs. Moreover, nonuniform curved bamboo-like MWCNTs with nozzles in the yield of 760% were obtained onto NiO/V2O3/MgO catalyst. Their diameter ranges from 25[Formula: see text]nm to 50[Formula: see text]nm. Results show that single-component catalyst promotes the growth of uniform and smaller nanotubes. Among the as-grown nanotubes, their specific surface area increases and average pores diameter reduces after the treatment with concentrated nitric acid at reflux and washing condition. The largest specific surface area (305[Formula: see text]m2/g) and average pores diameter (26[Formula: see text]m2/g) are processed to MWCNTs grown onto the NiO/Co2O3/MgO catalyst. MWCNTs with such large structural adsorption characteristics and purity of more than 99% obtained with yield 800% show potential use for preparation of nanocomposites as anode materials in lithium ion batteries.


2012 ◽  
Vol 519 ◽  
pp. 83-86 ◽  
Author(s):  
Guang Wu Liu ◽  
Xing Yuan Ni ◽  
Bin Zhou ◽  
Qiu Jie Yu

This paper deals with the synthesis of ultralow density silica aerogels using tetramethyl orthosilicate (TMOS) as the precursor via sol-gel process followed by supercritical drying using acetonitrile solvent extraction. Ultralow density silica aerogels with 6 mg/cc of density was made for the molar ratio by this method. The microstructure and morphology of the ultralow density silica aerogels was characterized by the specific surface area, SBET, SEM, and the pore size distribution techniques. The results show that the ultralow density silica aerogel has the high specific surface area of 812m2/g. Thermal conductivities at desired temperatures were analyzed by the transient plane heat source method. Thermal conductivity coefficients of silica aerogel monoliths changed from 0.024 to 0.043W/ (m K) as temperature increased to 400°C, revealed an excellent heat insulation effect during thermal process.


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