scholarly journals Synthesis of Monolithic TiO2 Aerogels With Relatively Low Shrinkage and Improved Formability Assisted by CTAB

2021 ◽  
Vol 8 ◽  
Author(s):  
Tingting Niu ◽  
Bin Zhou ◽  
Zehui Zhang ◽  
Jianming Yang ◽  
Xiujie Ji ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
Structure Property ◽  
Surface Areas ◽  
Polycondensation Process

Monolithic TiO2 aerogels without severe shrink were obtained by the sol-gel method with the addition of the surfactant cetyltrimethylammonium bromide (CTAB) to control the hydrolysis and polycondensation process and acetonitrile solvent as the solvent to improve the crystallinity. After CO2 supercritical drying, the shrinkage ratio of monolithic TiO2 aerogels modified by CTAB decreased by up to ∼26.9%, compared with the pure TiO2 aerogel. Their apparent densities were all lower than 300 g/cm3. X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier Transform infrared spectroscopy (FTIR) and BET Specific Surface Area Analysis were used to analyze the as-synthesized samples. The results revealed that all the samples were anatase-TiO2 phase with nanoporous network structures. The specific surface areas reached 250.2 m2/g confirmed by the BET (Brunaur–Emmett–Teller method) analysis. However, TiO2 aerogels without the addition of CTAB showed evident agglomeration and collapse of the network in comparison with CTAB-added samples. To further study the structure-property relationship, the photocatalysis performance of as-synthesized and 300°C-calcined aerogels was carried out contrastively. Interestingly, the influences of the CTAB adding amount of as-synthesized and calcined TiO2 aerogels are negative and positive, respectively, which is probably due to the synergistic effect of CTAB hindrance and grain refinement. Potentially, This kind of TiO2 aerogels assisted by CATB with low density, small shrinkage, improved formability, high specific surface area and fine crystalline grain may be applied in various applications, such as electrochemistry, photocatalysis, etc.

Preparation and Characterization of Ultralow Density Silica Aerogels by Acetonitrile Supercritical Drying

2012 ◽  
Vol 519 ◽  
pp. 83-86 ◽  
Author(s):  
Guang Wu Liu ◽  
Xing Yuan Ni ◽  
Bin Zhou ◽  
Qiu Jie Yu
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Silica Aerogel ◽  
Sol Gel ◽  
Supercritical Drying ◽  
Silica Aerogels ◽  
High Specific Surface Area ◽  
Molar Ratio ◽  
Sol Gel Process

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.

Synthesis and Structural Characterization of SiO2-Al2O3 Xerogels

2007 ◽  
Vol 336-338 ◽  
pp. 2286-2289
Author(s):  
Fei He ◽  
Xiao Dong He ◽  
Yao Li
Keyword(s):  
Structural Change ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
Nitrogen Adsorption ◽  
Mesoporous Structure ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
Molar Ratio

Low-density xSiO2-(1-x)Al2O3 xerogels with x=0.9, 0.8, 0.7, 0.6 (mole fractions) were prepared by sol-gel and non-supercritical drying. Silica alkogels, which were the framework of binary composite materials, formed from tetraethyl orthosilicate (TEOS) by hydrolytic condensation with a molar ratio of TEOS: H2O: alcohol: hydrochloric acid: ammonia =1: 4: 10: 7.5×10-4: 0.0375. Aluminum hydroxide derived from Al(NO3)3·9H2O and NH4OH acting in the alcohol solution under the condition of catalyst. After filtrating and washing, the precipitation was mixed into silica sols to form SiO2-Al2O3 mixed oxide gels with different silicon and aluminum molar ratio. The structural change and crystallization of the binary xerogels were investigated after heat treatment at 600 for 2 h by the means of X-ray diffraction. Nitrogen adsorption experiment was performed to estimate specific surface area, porous volume and pore size distribution. The structural change of xerogels was observed by FT-IR spectroscopy. The resulting mixed xerogels possess of mesoporous structure which is characteristic of cylindrical pores, high specific surface area of 596-863 m2/g and a relatively narrow pore distribution of 2.8-30 nm. Al2O3 is introduced into the SiO2 phase and some of Al-O-Si bonds form.

Rapid preparation process, structure and thermal stability of lanthanum doped alumina aerogels with a high specific surface area

RSC Advances ◽  
2016 ◽  
Vol 6 (31) ◽  
pp. 26271-26279 ◽  
Author(s):  
Jingfeng Yang ◽  
Qihua Wang ◽  
Tingmei Wang ◽  
Yongmin Liang
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
Rapid Preparation ◽  
Alumina Aerogels ◽  
Process Structure ◽  
Thermal Stability Of

In this study, we developed a new and rapid preparation method of alumina aerogels based on the sol–gel method and supercritical drying technique and prepared alumina aerogels with high specific surface area.

Preparation of CuO-CoO-MnO/SiO2 Nanocomposite Aerogels and the Effect of Synthesis Conditions on Gelation

2010 ◽  
Vol 148-149 ◽  
pp. 920-923
Author(s):  
Yue Qing Zhao ◽  
Ying Hua Liang ◽  
Feng Feng Li ◽  
Hong Ping Chen ◽  
Xin Hua Liu ◽  
...  
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
Synthesis Conditions ◽  
Sol Gel Process ◽  
Bet Method

CuO-CoO-MnO/SiO2 nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as transition metal sources via sol-gel process and supercritical drying (SCD) technique. The effect of synthesis conditions on gelation was investigated. The composition of the nanocomposite aerogels was characterized by electron dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The specific surface area of the nanocomposite aerogels was determined by the Brunauer-Emmett-Teller (BET) method. The results show that the range of optimal temperature for gelation is 30-45 °C, and the pH is 3.0-4.5. CuO-CoO-MnO/SiO2 nanocomposite aerogels are porous with a specific surface area of 384.9-700.6 m2/g. Compared to CO2 SCD, ethanol SCD is even favorable to the formation of aerogel with high specific surface area. The transition metals content in the nanocomposite aerogels can be controlled to be 0.71-13.77 at.%.

Alumina aerogel catalysts prepared by two supercritical drying methods used in methane combustion

1995 ◽  
Vol 10 (6) ◽  
pp. 1424-1428 ◽  
Author(s):  
Yasuyuki Mizushima ◽  
Makoto Hori
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Methane Combustion ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
The Other ◽  
Drying Methods ◽  
Alumina Aerogel ◽  
Lower Temperature

Palladium-supported alumina aerogels were prepared by two different supercritical drying methods. In one method, an alumina wet gel was dried under supercritical conditions of ethanol in an autoclave. In the other, the aerogel was supercritically dried by extracting ethanol using carbon dioxide in an extractor. The Pd-supported alumina aerogel prepared in the autoclave exhibited a high specific surface area of 112.8 m2/g after firing at 1200 °C for 5 h, while the other had a specific surface area of only 5.2 m2/g due to α-alumina transformation. Their catalytic properties for methane combustion were measured. The Pd-supported alumina aerogel prepared in the autoclave combusts methane perfectly at 50–60 °C lower temperature than the other. Palladium particles on the alumina aerogel prepared in the autoclave contained palladium oxide, while those prepared in the CO2 extractor contained only palladium metal.

Synthesis and Characterization of Porous Mo-W Oxide Nanostructures

2008 ◽  
Vol 8 (12) ◽  
pp. 6445-6450
Author(s):  
F. Paraguay-Delgado ◽  
Y. Verde ◽  
E. Cizniega ◽  
J. A. Lumbreras ◽  
G. Alonso-Nuñez
Keyword(s):  
Electron Microscopy ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Synthesis Method ◽  
Atomic Ratio ◽  
High Specific Surface Area ◽  
X Ray Diffraction ◽  
Transmission Electron ◽  
Before And After

The present study reports the synthesis method, microstructure characterization, and thermal stability of nanostructured porous mixed oxide (MoO3-WO3) at 550 and 900 °C of annealing. The material was synthesized using a hydrothermal method. The precursor was prepared by aqueous solution using ammonium heptamolibdate and ammonium metatungstate, with an atomic ratio of Mo/W = 1. The pH was adjusted to 5, and then the solution was transferred to a teflon-lined stainless steel autoclave and heated at 200 °C for 48 h. The resultant material was washed using deionized water. The specific surface area, morphology, composition, and microstructure before and after annealing were studied by N2 physisorption, scanning electron microscopy (SEM), analytical transmission electron microscopy (TEM), and X-Ray diffraction (XRD). The initial synthesized materials showed low crystallinity and high specific surface area around (141 m2/g). After thermal annealing the material showed higher crystallinity and diminished its specific surface area drastically.

Preparation and Characterization of Phloroglucinol-Resorcinol-Formaldehyde Carbon Aerogels

2013 ◽  
Vol 423-426 ◽  
pp. 523-527
Author(s):  
Xuan Liu ◽  
Zhen Fa Liu ◽  
Hao Lin Fu ◽  
Rui He ◽  
Li Hui Zhang
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
High Specific Surface Area ◽  
Carbon Aerogels ◽  
Resorcinol Formaldehyde ◽  
Sol Gel Process ◽  
Solvent Replacement ◽  
Organic Aerogels

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.

CVD Synthesis of Multi-Walled Carbon Nanotubes onto Different Catalysts at Low Temperature

NANO ◽  
2018 ◽  
Vol 13 (04) ◽  
pp. 1850036 ◽  
Author(s):  
Guiqiang Diao ◽  
Hao Li ◽  
Hao Liang ◽  
Iryna Ivanenko ◽  
Tetiana Dontsova ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Carbon Nanotubes ◽  
Low Temperature ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
Lithium Ion ◽  
Multi Walled Carbon Nanotubes ◽  
Walled Carbon Nanotubes

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.

Novel Al2O3–SiO2composite aerogels with high specific surface area at elevated temperatures with different alumina/silica molar ratios prepared by a non-alkoxide sol–gel method

RSC Advances ◽  
2016 ◽  
Vol 6 (7) ◽  
pp. 5611-5620 ◽  
Author(s):  
Xiaodong Wu ◽  
Gaofeng Shao ◽  
Xiaodong Shen ◽  
Sheng Cui ◽  
Ling Wang
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Elevated Temperatures ◽  
Inorganic Salt ◽  
Sol Gel ◽  
High Specific Surface Area ◽  
Gel Method ◽  
Molar Ratios ◽  
Composite Aerogels

We have developed a new sol–gel route to synthesise Al2O3–SiO2composite aerogels with different alumina/silica (Al/Si) molar ratios using an inexpensive inorganic salt.

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