Effect of pH, Molar Ratio of Fuel to Nitrates and Calcination Temperature on the Glycine-Nitrate Synthesis of Nano CoAl2O4

2010 ◽  
Vol 68 ◽  
pp. 176-181 ◽  
Author(s):  
Seyyed Hamid Jazayeri ◽  
Federica Bondioli ◽  
Shiva Salem ◽  
Ali Allahverdi ◽  
Mansoor Shirvani ◽  
...  

In this research, solution-based combustion synthesis is applied to prepare the spinel CoAl2O4 pigment from precursor solution of Al(NO3)3 .9H2O, Co(NO3)2 .6H2O and glycine. Effect of pH values (2.5, 7, 10.5), molar ratio of fuel to metal nitrates in the precursor solutions (1.5, 2) and subsequent calcination temperature (800, 1000, 1200 °C) on the powder characteristics are described. Gel formation, morphologies, specific surface area and colour of the powder are characterized using DTA/TG, XRD, TEM, BET and UV-Vis. The results indicate that the crystalline spinel CoAl2O4 is formed at all different Gl/(metal nitrates) molar ratios, pH and temperatures and higher temperature promote the increase of the crystallite size. According to TEM figures most of the particles calcined at 800 and 1000 °C has sizes less than 50 and 100 nm, respectively. Corresponding to results of BET experiment, specific surface area has its maximum values at pH 7 and decreases with increasing of temperature. Finally, colorability test indicates the complete stability of the synthesized powder in the glass matrix.

Materials ◽  
2019 ◽  
Vol 12 (23) ◽  
pp. 3862 ◽  
Author(s):  
Fangtong Xie ◽  
Emanuel Ionescu ◽  
Marcela Arango-Ospina ◽  
Ralf Riedel ◽  
Aldo R. Boccaccini ◽  
...  

In the present work, Ca-containing silicon oxycarbides (SiCaOC) with varying Ca content have been synthesized via sol-gel processing and thermal treatment in inert gas atmosphere (pyrolysis). It has been shown that the as-prepared SiCaOC materials with low Ca loadings (Ca/Si molar ratios = 0.05 or 0.12) were X-ray amorphous; their glassy network contains Q3 sites, indicating the presence of Ca2+ at non-bridging-oxygen sites. SiCaOC with high Ca content (i.e., Ca/Si molar ratio = 0.50) exhibits the presence of crystalline calcium silicate (mainly pseudowollastonite). Furthermore, it has been shown that the incorporation of Ca into the SiOC glassy network has a significant effect on its porosity and specific surface area. Thus, the as-prepared Ca-free SiOC material is shown to be non-porous and having a specific surface area (SSA) of 22.5 m2/g; whereas SiCaOC with Ca/Si molar ratio of 0.05 exhibits mesoporosity and a SSA value of 123.4 m2/g. The further increase of Ca content leads to a decrease of the SSA and the generation of macroporosity in SiCaOC; thus, SiCaOC with Ca/Si molar ratio of 0.12 is macroporous and exhibits a SSA value of 39.5 m2/g. Bioactivity assessment in simulated body fluid (SBF) confirms the hydroxyapatite formation on all SiCaOC samples after seven days soaking, unlike the relatively inert ternary silicon oxycarbide reference. In particular, SiCaOC with a Ca/Si molar ratio of 0.05 shows an increased apatite forming ability compared to that of SiCaOC with Ca/Si molar ratio of 0.12; this difference is considered to be a direct consequence of the significantly higher SSA of the sample with the Ca/Si ratio of 0.05. The present work indicates two effects of Ca incorporation into the silicon oxycarbide glassy network on its bioactivity: Firstly, Ca2+ is shown to contribute to the slight depolymerization of the network, which clearly triggers the hydroxyapatite formation (compare the bioactive behavior of SiOC to that of SiCaOC with Ca/Si molar ratio 0.12 upon SBF exposure); secondly, the Ca2+ incorporation seems to strongly affect the porosity and SSA in the prepared SiCaOC materials. There is an optimum of Ca loading into the silicon oxycarbide glassy network (at a Ca/Si molar ration of 0.05), which provides mesoporosity and reaches maximum SSA, both highly beneficial for the bioactive behavior of the materials. An increase of the Ca loading leads, in addition to the crystallization of calcium silicates, to a coarsening of the pores (i.e., macroporosity) and a significant decrease of the SSA, both negatively affecting the bioactivity.


Materials ◽  
2021 ◽  
Vol 14 (17) ◽  
pp. 4963
Author(s):  
Yongfu Wu ◽  
Hong Li ◽  
Xue Bian ◽  
Wenyuan Wu ◽  
Zhenfeng Wang ◽  
...  

Green and short preparation of CeO2 nanoparticles with large specific surface area from rare earth extraction (CeCl3) was successfully achieved by spray pyrolysis (SP). In this method, a precursor solution is first prepared by mixing CeCl3, C6H8O, and H2O in the requisite quantities. Subsequently, the precursor consisting of a mixture of CeO2 and C was obtained by SP method by using the precursor solution. Finally, the calcination at 500 °C~800 °C in air for two hours to transform the precursor to CeO2 nanoparticles. Thermodynamic analysis and experimental studies were performed to determine the optimal SP temperature and citric acid amount. The results indicated that the maximum specific surface area (59.72 m2/g) of CeO2 nanoparticles were obtained when the SP temperature was 650 °C and the molar ratio of citric acid to CeCl3 was 1.5.


2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Yosep Han ◽  
Hyung-Seok Kim ◽  
Hyunjung Kim

The degradation efficiency of methylene blue by TiO2nanoparticles, which were synthesized under different synthesis conditions (i.e., molar ratio of water and titanium tetraisopropoxide (TTIP), pH, and calcination temperature) in a sol-gel process, was systematically investigated. The results showed that increasing the molar ratio of water and TTIP led to the enhanced photocatalytic activity of TiO2nanoparticles, which were likely attributed to the increased specific surface area of TiO2nanoparticles synthesized with high molar ratio. The results were supported by the relative increase in the size of interaggregated pores of the aggregated TiO2nanoparticles. The best photocatalytic activity of TiO2nanoparticles was observed at acidic synthesis conditions; however, the results were not consistent with physical properties for the crystallinity and the crystallite size of TiO2nanoparticles but rather explained by the presence of abundant hydroxyl groups and water molecules existing on the surface of TiO2under acidic synthesis environments. Furthermore, methylene blue degradation experiments revealed that the photocatalytic activity of TiO2nanoparticles was maximized at the calcination temperature of 700°C. The trend was likely due to the combined effect of the anatase crystallinity which showed the highest value at 700°C and the crystallite size/specific surface area which did not excessively increase up to 700°C.


2017 ◽  
Vol 36 (1-2) ◽  
pp. 247-269 ◽  
Author(s):  
Armin Taheri ◽  
Ensieh Ganji Babakhani ◽  
Jafar Towfighi

In this study hydrothermal method was used to synthesize MIL-53(Al) (MIL stands for Materials Institute of Lavoisier). Plackett–Burman (P–B) as an experimental design method was applied to investigate the effect of synthesis and activation conditions on specific surface area, relative crystallinity, and production yield of MIL-53(Al) synthesis. Some parameters such as ligand-to-metal molar ratio, synthesis time, synthesis temperature, calcination temperature, and calcination time were selected as the variables. The Brunauer–Emmett–Teller (BET) technique was used in order to estimate the specific surface area of samples while the relative crystallinity of the samples was estimated by comparing their X-Ray Diffraction (XRD) pattern. The morphology of the samples was investigated by field emission scanning electron microscopy. The yield of final products was determined based on organic ligands. The results revealed the significant effect of synthesis temperature on BET surface area, particle size, yield, and crystallinity. The calcination temperature has significant positive effect on BET and crystallinity. Also, the negative significant effect of molar ratio on yield was concluded from the results. However, negligible effect of synthesis and calcination time on the properties of prepared materials were observed. Furthermore, separation capability of a selected sample for carbon dioxide (CO2) and methane (CH4) was measured. Pure gas adsorption data were successfully fitted to Langmuir, Sips, and Toth models. The selected sample provided high adsorption capacity for both gases. The binary adsorption of gases was also investigated based on extended Langmuir equations and the ideal adsorbed solution theory (IAST) models. Comparing the experimental and models data indicated good agreement between the IAST model and experiments. Finally, high CO2/CH4 selectivity of 7.6 was obtained experimentally for the CO2/CH4 molar ratio of 0.2/0.8.


2021 ◽  
Vol 1036 ◽  
pp. 130-136
Author(s):  
Ting Qun Tan ◽  
Lei Geng ◽  
Yan Lin ◽  
Yan He

In order to prepare carbon nanotubes with high specific surface area, small diameter, low resistivity, high purity and high catalytic activity, the Fe-Mo/Al2O3 catalyst was prepared based on the microreactor. The influence of different Fe/Al molar ratios on the catalyst and the carbon nanotubes prepared was studied through BET, SEM, TEM and other detection methods. Studies have shown that the pore structure of the catalyst is dominated by slit pores at a lower Fe/Al molar ratio. The catalytic activity is the highest when the Fe/Al molar ratio is 1:1, reaching 74.1%. When the Fe/Al molar ratio is 1:2, the catalyst has a higher specific surface area, the maximum pore size is 8.63 nm, and the four-probe resistivity and ash content of the corresponding carbon nanotubes are the lowest. The higher the proportion of aluminum, the higher the specific surface area of the catalyst and the carbon nanotubes, and the finer the diameter of the carbon nanotubes, which gradually tends to relax. The results show that when the Fe/Al molar ratio is 1:2, although the catalytic activity of the catalyst is not the highest, the carbon nanotubes prepared have the best performance.


Paliva ◽  
2020 ◽  
pp. 155-161
Author(s):  
Tomáš Hlinčík ◽  
Veronika Šnajdrová ◽  
Veronika Kyselová

Alumina is commonly used in industrial practice as a catalyst support and it is made from boehmite. Depending on the calcination temperature, this mineral is transformed into various crystalline modifications which have different physical and chemical properties. For this reason, the following parameters were determined at different calcination temperatures: length, width, material hardness, specific surface area and total pore volume. The results show that with increasing calcination temperature there have been significant changes which may be important when using the material as a catalyst support, e.g. in the preparation of catalysts or in the design of cat-alytic reactors. The specific surface area, which decreases in the temperature range 450–800 °C, is an important parameter for the preparation of catalysts, so it is appropriate to choose a temperature of 600 °C, when the specific surface area is above 200 m2·g-1. The effect of calcination temperature on the structural transitions of boehmite was also monitored. The results showed that γ-Al2O3 has the most suitable properties as a catalyst sup-port in the temperature range 450–800 °C.


2005 ◽  
Vol 284-286 ◽  
pp. 365-368 ◽  
Author(s):  
Yin Zhang ◽  
Yoshiyuki Yokogawa ◽  
Tetsuya Kameyama

The effect of different particle sizes on the flexural strength and microstructure of three different types of hydroxyapatite (HAp) powders was studied. The powder characteristics of laboratory synthesized HAp powder (Lab1 and Lab2) were obtained through a wet milling method, and the median particle size and the specific surface area of powders are different with the dryness period. The median particle sizes of Lab1 and Lab2 are 0.34 µm and 0.74 µm, and the specific surface areas of Lab1 and Lab2 are 38.01 m2/g and 19.77 m2/g. The commercial HAp had median particle size of 1.13 µm and specific surface area of 11.62m2/g. The different powder characteristics affected the slip characteristics, and the flexural strength and microstructure of the sintered porous HAp bodies are also different. The optimum value for the minimum viscosity in these present HAp slip with respect to its solid loading and the optimum amount of the deflocculant were investigated. The flexural strengths of the porous HAp ceramics prepared by heating at 1200°C for 3 hrs in air were 17.59 MPa for Lab1 with a porosity of 60.48%, 10.51 MPa for Lab2 with a porosity of 57.75%, and 3.92 MPa for commercial HAp with a porosity of 79.37%.


2016 ◽  
Vol 721 ◽  
pp. 172-176 ◽  
Author(s):  
Jana Vecstaudza ◽  
Janis Locs

Amorphous and low crystalline calcium phosphates are prospective candidates for bone implant manufacturing. Amorphous calcium phosphate (ACP) preparation technologies could be improved in terms of specific surface area (SSA) of obtained products. Current study is dedicated to the effect of synthesis temperature and Ca and P molar ratios (Ca/P) on SSA of ACP. Higher SSA can improve bioactivity of biomaterials. ACP was characterized by XRD, FT-IR, SEM and BET N2 adsorption techniques. Spherical nanoparticles (<45 nm in size) were obtained independently of initial Ca/P ratio and synthesis temperature. For the first time comparison of SSA was shown for ACP obtained at different temperatures (0 °C and 20 °C) and Ca/P molar ratios (1.5, 1.67 and 2.2).


2020 ◽  
Vol 998 ◽  
pp. 78-83
Author(s):  
Yi Yi Zaw ◽  
Du Ang Dao Channei ◽  
Thotsaphon Threrujirapapong ◽  
Wilawan Khanitchaidecha ◽  
Auppatham Nakaruk

Titanium dioxide (TiO2) is known as one of the widely used catalysts in photocatalysis process. Recently, the photocatalysis of TiO2 has been implied in water purification and treatment, particularly dyes and organic compounds degradations. Naturally, the TiO2 can be found in three phases including anatase, rutile and brookite; each phase has its own specific properties such as grain size, stability and band gap energy. In this work, the effect of calcination temperature on the structure, morphology and photocatalytic activity were investigated. The data suggested that the anatase/rutile ratio of TiO2 can be controlled through the calcination process. The phase transformation data strongly indicated the liner function between percentage of rutile phase and calcination temperature. The BET analysis provided the consistent data with XRD patterns by showing that the specific surface area was decreased by increasing calcination temperature. The photodegradation of methylene blue under UV irradiation proved that the mixed phase of anatase/rutile ratio at 78.5/21.5 provided the highest photocatalytic activity. The phase composition ratio can influence the nanoparticles properties including band gap, specific surface area and energy band structure. Therefore, the control of anatase/rutile ratio was an alternative to enhance the photocatalytic activity of TiO2 nanoparticles for dyes and organic compounds degradations.


2011 ◽  
Vol 412 ◽  
pp. 361-364
Author(s):  
Wei Jun Zhang ◽  
Yuan Feng Huang ◽  
Li Shen ◽  
Jun Liu ◽  
Xiao Qing Luo ◽  
...  

A series of Ba-Al-O/NSR supports were prepared by co-precipitation in this work. The effect of Al/Ba atomic ratio and calcination temperature on the structure and texture of the supports was investigated carefully. The XRD spectra show that Ba is mainly exist in the form of BaAl2O4, and Al exists in Al2O3. The results of SBET indicate that the supports possess relative high specific surface area (70~150 m2/g). The effect of different parameters on the process of supports synthesized was investigated carefully. The results show that the structure and specific surface area of support is significantly depended on calcination temperature.


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