scholarly journals Preparation of TiO2 and Fe-TiO2 with an Impinging Stream-Rotating Packed Bed by the Precipitation Method for the Photodegradation of Gaseous Toluene

Nanomaterials ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 1173 ◽  
Author(s):  
Guangping Zeng ◽  
Qiaoling Zhang ◽  
Youzhi Liu ◽  
Shaochuang Zhang ◽  
Jing Guo

Nano-TiO2 has always been one of the most important topics in the research of photocatalysts due to its special activity and stability. However, it has always been difficult to obtain nano-TiO2 with high dispersion, a small particle size and high photocatalytic activity. In this paper, nano-TiO2 powder was prepared by combining the high-gravity technique and direct precipitation method in an impinging stream-rotating packed bed (IS-RPB) reactor followed by Fe3+ in-situ doping. TiOSO4 and NH3·H2O solutions were cut into very small liquid microelements by high-speed rotating packing, and the mass transfer and microscopic mixing of the nucleation and growth processes of nano-TiO2 were strengthened in IS-RPB, which was beneficial to the continuous production of high quality nano-TiO2. Pure TiO2 and iron-doped nano-TiO2 (Fe-TiO2) were obtained in IS-RPB and were investigated by means of X-ray diffraction (XRD), Raman, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS) and Brunauer–Emmett–Teller (BET) analysis, which found that pure TiO2 had a particle size of about 12.5 nm, good dispersibility and a complete anatase crystal at the rotating speed of packing of 800 rpm and calcination temperature of 500 °C. The addition of Fe3+ did not change the crystalline structure of TiO2. Iron was highly dispersed in TiO2 without the detection of aggregates and was found to exist in a positive trivalent form by XPS. With the increase of iron doping, the photoresponse range of TiO2 to visible light was broadened from 3.06 eV to 2.26 eV. The degradation efficiency of gaseous toluene by Fe-TiO2 under ultraviolet light was higher than that of pure TiO2 and commercial P25 due to Fe3+ effectively suppressing the recombination of TiO2 electrons and holes; the highest efficiency produced by 1.0% Fe-TiO2 was 95.7%.

Nanomaterials ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 263 ◽  
Author(s):  
Xiaojing Ren ◽  
Youzhi Liu ◽  
Longxin Miao

This research established a novel method for the preparation of pseudo-boehmite (PB) via a continuous carbonation of CO2 gas and a NaAlO2 solution in a cross-flow rotating packed bed (CF-RPB). In the CF-RPB, the NaAlO2 solution can be sheared into fine liquid filaments and droplets, and react in full contact with the CO2 gas. Effects of synthesis parameters, including the concentration of the NaAlO2 solution, the gas–liquid ratio, the rotating speed of the CF-RPB, and the final pH of the solution on the crystal structure of PB, were fully investigated. A series of characterizations, including X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) analysis, were carried out to explain the evaluation results and to find the relationship between PB properties and the synthetic conditions. The results showed that PB with a high specific surface area (495 m2/g) and large pore volume (2.125 cc/g) can be obtained when the concentration of the NaAlO2 solution was 0.1 mol/L, the gas–liquid ratio was 3:1, the rotating speed of RPB was 600 rpm, and the final pH was around 10.5. PB obtained by this method had a higher quality compared with that using a stirred tank reactor. Moreover, the continuous carbonation can be efficiently batch-produced, which provided a new idea for an industrial application.


2018 ◽  
Vol 24 (8) ◽  
pp. 5640-5644
Author(s):  
B Sreenivasulu ◽  
S. Venkatramana Reddy ◽  
P. Venkateswara Reddy

Pure ZnS and 3 mol% of Ni doped ZnS nano powders are prepared by chemical co-precipitation method. Properties of ZnS: Ni2+ nanoparticles are studied by X-ray diffraction Spectra (XRD), Raman spectroscopy (RS), Photoluminescence (PL), Absorption Spectra, Scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDAX), Transmission electron microscopy (TEM) and Vibrating sample magnetometer (VSM). From XRD data, it conform the structure of ZnS, and particle size of pure and Ni doped ZnS data indicates the incorporation of Ni2+ in ZnS nanocrystal lattice. Raman spectra for pure and Ni doped samples exhibited vibrational modes confirm the structure of ZnS. Photoluminescence spectra reveal that the emission peaks are in UV and visible regions; this is confirming the absorption spectra. SEM micrographs show spherical morphology, and chemical compositions of samples are in stoichiometric proportions. TEM micro graphs show the spherical surface morphology and average particle size for pure and Ni2+ doped nanoparticles are in the range of 2–3 nm, this is good agreement with XRD results. M–H curves from VSM show room temperature ferromagnetism.


2008 ◽  
Vol 368-372 ◽  
pp. 635-637
Author(s):  
Jian Feng Huang ◽  
Li Yun Cao ◽  
Jian Peng Wu ◽  
Hai Yan He

Nanocrystalline Y2BaCuO5 was prepared by a co-precipitation method with aid of ultrasonic irradiation using Y2O3, CuCl2 and BaCl2 as source materials. The crystallization and morphology of the prepared nanoparticles were characterized by X-ray diffraction and transmission electron microscopy. Results showed that Y2BaCuO5 monophase can be prepared at 900°C with NaOH + NaCO3 mixture as precipitator. Particle size of Y2BaCuO5 crystallites decreases with the increase of sonicating power. Around 30 nm Y2BaCuO5 crystallites could be achieved when sonicating power increased to 300 W.


Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 25
Author(s):  
Chukwuka Bethel Anucha ◽  
Ilknur Altin ◽  
Emin Bacaksız ◽  
Tayfur Kucukomeroglu ◽  
Masho Hilawie Belay ◽  
...  

Abatement of contaminants of emerging concerns (CECs) in water sources has been widely studied employing TiO2 based heterogeneous photocatalysis. However, low quantum energy yield among other limitations of titania has led to its modification with other semiconductor materials for improved photocatalytic activity. In this work, a 0.05 wt.% CuWO4 over TiO2 was prepared as a powder composite. Each component part synthesized via the sol-gel method for TiO2, and CuWO4 by co-precipitation assisted hydrothermal method from precursor salts, underwent gentle mechanical agitation. Homogenization of the nanopowder precursors was performed by zirconia ball milling for 2 h. The final material was obtained after annealing at 500 °C for 3.5 h. Structural and morphological characterization of the synthesized material has been achieved employing X-ray diffraction (XRD), Fourier transform infra-red (FTIR) spectroscopy, Brunauer–Emmett–Teller (BET) N2 adsorption–desorption analysis, Scanning electron microscopy-coupled Energy dispersive X-ray spectroscopy (SEM-EDS), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and UV-Vis diffuse reflectance spectroscopy (UV-vis DRS) for optical characterization. The 0.05 wt.% CuWO4-TiO2 catalyst was investigated for its photocatalytic activity over carbamazepine (CBZ), achieving a degradation of almost 100% after 2 h irradiation. A comparison with pure TiO2 prepared under those same conditions was made. The effect of pH, chemical scavengers, H2O2 as well as contaminant ion effects (anions, cations), and humic acid (HA) was investigated, and their related influences on the photocatalyst efficiency towards CBZ degradation highlighted accordingly.


Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 76
Author(s):  
Chelladurai Karuppiah ◽  
Balamurugan Thirumalraj ◽  
Srinivasan Alagar ◽  
Shakkthivel Piraman ◽  
Ying-Jeng Jame Li ◽  
...  

Developing a highly stable and non-precious, low-cost, bifunctional electrocatalyst is essential for energy storage and energy conversion devices due to the increasing demand from the consumers. Therefore, the fabrication of a bifunctional electrocatalyst is an emerging focus for the promotion and dissemination of energy storage/conversion devices. Spinel and perovskite transition metal oxides have been widely explored as efficient bifunctional electrocatalysts to replace the noble metals in fuel cell and metal-air batteries. In this work, we developed a bifunctional catalyst for oxygen reduction and oxygen evolution reaction (ORR/OER) study using the mechanochemical route coupling of cobalt oxide nano/microspheres and carbon black particles incorporated lanthanum manganite perovskite (LaMnO3@C-Co3O4) composite. It was synthesized through a simple and less-time consuming solid-state ball-milling method. The synthesized LaMnO3@C-Co3O4 composite was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, Brunauer-Emmett-Teller (BET) analysis, X-ray diffraction spectroscopy, and micro-Raman spectroscopy techniques. The electrocatalysis results showed excellent electrochemical activity towards ORR/OER kinetics using LaMnO3@C-Co3O4 catalyst, as compared with Pt/C, bare LaMnO3@C, and LaMnO3@C-RuO2 catalysts. The observed results suggested that the newly developed LaMnO3@C-Co3O4 electrocatalyst can be used as a potential candidate for air-cathodes in fuel cell and metal-air batteries.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 825
Author(s):  
Saman Sargazi ◽  
Mohammad Reza Hajinezhad ◽  
Abbas Rahdar ◽  
Muhammad Nadeem Zafar ◽  
Aneesa Awan ◽  
...  

In this research, tin ferrite (SnFe2O4) NPs were synthesized via hydrothermal route using ferric chloride and tin chloride as precursors and were then characterized in terms of morphology and structure using Fourier-transform infrared spectroscopy (FTIR), Ultraviolet–visible spectroscopy (UV-Vis), X-ray power diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) method. The obtained UV-Vis spectra was used to measure band gap energy of as-prepared SnFe2O4 NPs. XRD confirmed the spinel structure of NPs, while SEM and TEM analyses disclosed the size of NPs in the range of 15–50 nm and revealed the spherical shape of NPs. Moreover, energy dispersive X-ray spectroscopy (EDS) and BET analysis was carried out to estimate elemental composition and specific surface area, respectively. In vitro cytotoxicity of the synthesized NPs were studied on normal (HUVEC, HEK293) and cancerous (A549) human cell lines. HUVEC cells were resistant to SnFe2O4 NPs; while a significant decrease in the viability of HEK293 cells was observed when treated with higher concentrations of SnFe2O4 NPs. Furthermore, SnFe2O4 NPs induced dramatic cytotoxicity against A549 cells. For in vivo study, rats received SnFe2O4 NPs at dosages of 0, 0.1, 1, and 10 mg/kg. The 10 mg/kg dose increased serum blood urea nitrogen and creatinine compared to the controls (P < 0.05). The pathology showed necrosis in the liver, heart, and lungs, and the greatest damages were related to the kidneys. Overall, the in vivo and in vitro experiments showed that SnFe2O4 NPs at high doses had toxic effects on lung, liver and kidney cells without inducing toxicity to HUVECs. Further studies are warranted to fully elucidate the side effects of SnFe2O4 NPs for their application in theranostics.


2019 ◽  
Vol 56 ◽  
pp. 17-27
Author(s):  
Van Dat Doan ◽  
Van Thuan Le ◽  
Hoang Sinh Le ◽  
Dinh Hien Ta ◽  
Hoai Thuong Nguyen

In this work, nanosized calcium deficient hydroxyapatite (nCDHA) was synthesized by the precipitation method, and then utilized as an adsorbent for removal of Fe (II), Cu (II), Ni (II) and Cr (VI) ions from aqueous solutions after characterizing it by various techniques as scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX) and BET method. A possible structure of synthesized nCDHA was proposed. The adsorption study indicated that the adsorption equilibrium is well fitted with Langmuir isotherm model with the maximum adsorption capacities followed the order of Fe (II) > Cu (II) > Ni (II) > Cr (VI) with the values of 137.23, 128.02, 83.19 and 2.92 mg/g, respectively. The ion-exchange mechanism was dominant for the adsorption of metal ions onto nCDHA at initial metal concentrations lower than 0.01 mol/L. Along with the ion-exchange mechanism, there was an additional precipitation occurred on the surface of nCDHA in the case of Fe (II) and Cu (II) at initial concentrations higher than 0.01 mol/L.


2011 ◽  
Vol 284-286 ◽  
pp. 684-687
Author(s):  
Chang Yu Li ◽  
Li Li Liu ◽  
Shou Xin Liu

Without using any templates or surfactants, flowerlike α-nickel hydroxide (Ni(OH)2) was successfully synthesized by homogeneous precipitation method. The prepared products were characterized by X-ray powder diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and N2 adsorption-desorption. The prepared Ni(OH)2 is α-phase with specific surface area of 245.0 m2/g and shows flowerlike structure with 4-6 um in diameter.


Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1712
Author(s):  
Appusamy Muthukrishnaraj ◽  
Salma Ahmed Al-Zahrani ◽  
Ahmed Al Otaibi ◽  
Semmedu Selvaraj Kalaivani ◽  
Ayyar Manikandan ◽  
...  

Towards the utilization of Cu2O nanomaterial for the degradation of industrial dye pollutants such as methylene blue and methyl orange, the graphene-incorporated Cu2O nanocomposites (GCC) were developed via a precipitation method. Using Hummers method, the grapheme oxide (GO) was initially synthesized. The varying weight percentages (1–4 wt %) of GO was incorporated along with the precipitation of Cu2O catalyst. Various characterization techniques such as Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), UV–visible diffused reflectance (UV-DRS), Raman spectroscopy, thermo gravimetric analysis (TGA), energy-dispersive X-ray analysis (EDX), and electro chemical impedance (EIS) were followed for characterization. The cabbage-like morphology of the developed Cu2O and its composites were ascertained from field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM). In addition, the growth mechanism was also proposed. The results infer that 2 wt % GO-incorporated Cu2O composites shows the highest value of degradation efficiency (97.9% and 96.1%) for MB and MO at 160 and 220 min, respectively. Further, its catalytic performance over visible region (red shift) was also enhanced to an appreciable extent, when compared with that of other samples.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


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