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Title: Microwave-Assisted Synthesis of Perovskite SrSnO 3 Nanocrystals in Ionic Liquids for Photocatalytic Applications

Abstract

Nanosized SrSnO 3 photocatalysts have been successfully synthesized by microwave synthesis in various ionic liquids (ILs) followed by a heat treatment process to optimize the materials’ crystallinity. The influence of the ILs with various cations such as 1-butyl-3-methylimidazolium ([C 4mim] +), 6-bis(3-methylimidazolium-1-yl)hexane ([C 6(mim) 2] 2+), butylpyridinium ([C 4Py] +), and tetradecyltrihexylphosphonium ([P 66614] +) and bis(trifluoromethanesulfonyl)amide ([Tf 2N] -) as the anion on the structure, crystallization, and morphology of the products was investigated. The samples were characterized by X-ray diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), surface area analysis by gas adsorption, X-ray photoelectron spectroscopy (XPS), diffuse reflectance UV–vis spectroscopy, and Raman and IR spectroscopy. According to structure characterization by XRD and Raman spectroscopy all samples crystallized phase-pure in the orthorhombic GdFeO 3 perovskite structure type. SEM reveals that, on the basis of the IL, the obtained SrSnO 3 nanoparticles exhibit different morphologies and sizes. Rod-shaped particles are formed in [C 4mim][Tf 2N], [C 6(mim) 2][Tf 2N] 2, and [P 66614][Tf 2N]. However, the particle dimensions and size distribution vary depending on the IL and range from quite thin and long needlelike particles with a narrow size distribution obtained in [P 66614][Tf 2N] to relatively larger particles withmore » a broader size distribution obtained in [C 6(mim) 2][Tf 2N] 2. In contrast, in [C 4Py][Tf 2N] nanospheres with a diameter of about 50 nm form. For these particles the highest photocatalytic activity was observed. Our investigations indicate that the improved photocatalytic activity of this material results from the synergistic effect of the relatively large surface area associated with nanosize and an appropriate energy band structure.« less

Authors:
 [1];  [2];  [3];  [4];  [4];  [4];  [5];  [1];  [2];  [3];  [6]
  1. Iowa State Univ., Ames, IA (United States). Dept. of Materials Science and Engineering. Center for Catalysis
  2. (United States)
  3. (Germany). Faculty of Chemistry and Biochemistry
  4. Ruhr Univ., Bochum (Germany). Faculty of Chemistry and Biochemistry
  5. (Germany). Inst. of Chemistry
  6. (Sweden). Dept. of Materials and Environmental Chemistry
Publication Date:
Research Org.:
Ames Lab., Ames, IA (United States); Ruhr Univ., Bochum (Germany); Iowa State Univ., Ames, IA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1399481
Report Number(s):
IS-J9378
Journal ID: ISSN 0020-1669
Grant/Contract Number:
AC02-07CH11358
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Volume: 56; Journal Issue: 12; Journal ID: ISSN 0020-1669
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Alammar, Tarek, Ames Lab., Ames, IA, Ruhr Univ., Bochum, Hamm, Ines, Grasmik, Viktoria, Wark, Michael, Univ. of Oldenburg, Mudring, Anja-Verena, Ames Lab., Ames, IA, Ruhr Univ., Bochum, and Stockholm Univ.. Microwave-Assisted Synthesis of Perovskite SrSnO3 Nanocrystals in Ionic Liquids for Photocatalytic Applications. United States: N. p., 2017. Web. doi:10.1021/acs.inorgchem.7b00279.
Alammar, Tarek, Ames Lab., Ames, IA, Ruhr Univ., Bochum, Hamm, Ines, Grasmik, Viktoria, Wark, Michael, Univ. of Oldenburg, Mudring, Anja-Verena, Ames Lab., Ames, IA, Ruhr Univ., Bochum, & Stockholm Univ.. Microwave-Assisted Synthesis of Perovskite SrSnO3 Nanocrystals in Ionic Liquids for Photocatalytic Applications. United States. doi:10.1021/acs.inorgchem.7b00279.
Alammar, Tarek, Ames Lab., Ames, IA, Ruhr Univ., Bochum, Hamm, Ines, Grasmik, Viktoria, Wark, Michael, Univ. of Oldenburg, Mudring, Anja-Verena, Ames Lab., Ames, IA, Ruhr Univ., Bochum, and Stockholm Univ.. 2017. "Microwave-Assisted Synthesis of Perovskite SrSnO3 Nanocrystals in Ionic Liquids for Photocatalytic Applications". United States. doi:10.1021/acs.inorgchem.7b00279. https://www.osti.gov/servlets/purl/1399481.
@article{osti_1399481,
title = {Microwave-Assisted Synthesis of Perovskite SrSnO3 Nanocrystals in Ionic Liquids for Photocatalytic Applications},
author = {Alammar, Tarek and Ames Lab., Ames, IA and Ruhr Univ., Bochum and Hamm, Ines and Grasmik, Viktoria and Wark, Michael and Univ. of Oldenburg and Mudring, Anja-Verena and Ames Lab., Ames, IA and Ruhr Univ., Bochum and Stockholm Univ.},
abstractNote = {Nanosized SrSnO3 photocatalysts have been successfully synthesized by microwave synthesis in various ionic liquids (ILs) followed by a heat treatment process to optimize the materials’ crystallinity. The influence of the ILs with various cations such as 1-butyl-3-methylimidazolium ([C4mim]+), 6-bis(3-methylimidazolium-1-yl)hexane ([C6(mim)2]2+), butylpyridinium ([C4Py]+), and tetradecyltrihexylphosphonium ([P66614]+) and bis(trifluoromethanesulfonyl)amide ([Tf2N]-) as the anion on the structure, crystallization, and morphology of the products was investigated. The samples were characterized by X-ray diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), surface area analysis by gas adsorption, X-ray photoelectron spectroscopy (XPS), diffuse reflectance UV–vis spectroscopy, and Raman and IR spectroscopy. According to structure characterization by XRD and Raman spectroscopy all samples crystallized phase-pure in the orthorhombic GdFeO3 perovskite structure type. SEM reveals that, on the basis of the IL, the obtained SrSnO3 nanoparticles exhibit different morphologies and sizes. Rod-shaped particles are formed in [C4mim][Tf2N], [C6(mim)2][Tf2N]2, and [P66614][Tf2N]. However, the particle dimensions and size distribution vary depending on the IL and range from quite thin and long needlelike particles with a narrow size distribution obtained in [P66614][Tf2N] to relatively larger particles with a broader size distribution obtained in [C6(mim)2][Tf2N]2. In contrast, in [C4Py][Tf2N] nanospheres with a diameter of about 50 nm form. For these particles the highest photocatalytic activity was observed. Our investigations indicate that the improved photocatalytic activity of this material results from the synergistic effect of the relatively large surface area associated with nanosize and an appropriate energy band structure.},
doi = {10.1021/acs.inorgchem.7b00279},
journal = {Inorganic Chemistry},
number = 12,
volume = 56,
place = {United States},
year = 2017,
month = 6
}

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  • Nanocrystalline Sr 1–xBa xSnO 3 (x = 0, 0.2, 0.4, 0.8, 1) perovskite photocatalysts were prepared by microwave synthesis in an ionic liquid (IL) and subsequent heat-treatment. The influence of the Sr/Ba substitution on the structure, crystallization, morphology, and photocatalytic efficiency was investigated and the samples were fully characterized. On the basis of X-ray diffraction results, as the Ba content in the SrSnO 3 lattice increases, a symmetry increase was observed from the orthorhombic perovskite structure for SrSnO 3 to the cubic BaSnO 3 structure. The analysis of the sample morphology by SEM reveals that the Sr 1–xBa xSnO 3more » samples favor the formation of nanorods (500 nm–5 μm in diameter and several micrometers long). The photophysical properties were examined by UV/Vis diffuse reflectance spectroscopy. The band gap decreases from 3.85 to 3.19 eV with increasing Ba 2+ content. Furthermore, the photocatalytic properties were evaluated for the hydroxylation of terephthalic acid (TA). The order of the activities for TA hydroxylation was Sr 0.8Ba 0.2SnO 3 > SrSnO 3 > BaSnO 3 > Sr 0.6Ba 0.4SnO 3 > Sr 0.2Ba 0.8SnO 3. Here, the highest photocatalytic activity was observed for Sr 0.8Ba 0.2SnO 3, and this can be attributed to the synergistic impacts of the modification of the crystal structure and morphology, the relatively large surface area associated with the small crystallite size, and the suitable band gap and band-edge position.« less
  • Graphical abstract: - Highlights: • Three kinds of CdS nanostructures have been controllably synthesized. • Ethanediamine acts as a phase and morphology controlling reagent. • Three CdS nanostructures display high visible light photocatalytic activities. • Cubic CdS-3 shows superior photocatalytic activity to the other hexagonal CdS. • The growth processes for fabrication of CdS nanocrystals are also discussed. - Abstract: Three kinds of CdS nanostructures, that is, hexagonal nanospheres (CdS-1), hierarchical caterpillar-fungus-like hexagonal nanorods (CdS-2) and hierarchical cubic microspheres (CdS-3), were controllably synthesized by a facile and one-pot microwave-assisted aqueous chemical method using ethanediamine as a phase and morphology controllingmore » reagent. The as-prepared products were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), UV–vis diffuse reflectance spectra (DRS) and photoluminescence (PL) spectra. The results show that CdS-1 is mainly composed of monodispersed hexagonal nanospheres with average diameters of about 100 nm; hexagonal CdS-2 has lengths in the range of 600–800 nm and diameters of 40–60 nm, assembled by nanoparticles about 20 nm in diameter; and CdS-3 is pure cubic microspheres with diameters in the range of 0.8–1.3 μm, aggregated by tiny nanograins with size of 5.8 nm. The band gap energies of CdS products were calculated to be 2.30, 2.31 and 2.24 eV observed from UV–vis DRS for CdS-1, CdS-2 and CdS-3, respectively. PL spectra of CdS samples showed that sphalerite CdS-3 possesses a very weak fluorescence, while wurtzite CdS-2 has a strongest green near-band edge emission (NBE) at 550 nm. The visible light photodegradation of methylene blue and rhodamine B in the presence of CdS photocatalysts illustrates that all of them display high photocatalytic activities. Significantly, the cubic CdS-3 exhibits more excellent photocatalytic behavior in degradation of organic dyes than the other hexagonal CdS, which is closely related to the phase and morphology structure of cubic CdS.« less
  • A simple microwave synthesis procedure has been developed for the single-crystalline perovskite nanocubes composed of bismuth ferrite (BiFeO{sub 3}). Typical nanocubes had sizes ranging from 50 to 200 nm. The single-crystalline nature of nanocubes was confirmed by high resolution transmission electron microscopy and selected area electron diffraction pattern. X-ray diffraction pattern showed the rhombohedral phase with R3c space group. The material showed photoinduced water oxidation activity in both photoelectrochemical and photocatalytic modes. It could become a useful material for photoelectrode and photocatalytic applications.
  • Highlights: • TiO{sub 2}: Li nanoparticles were synthesized via an ionic liquid-assisted hydrothermal method. • The doping of Li to anatase TiO{sub 2} affects the properties of the resultant product. • TiO{sub 2}: Li nanoparticles were used as a photocatalyst for the degradation of dye. • TiO{sub 2}: Li nanoparticles were used as sensor, and antibacterial agent. • TiO{sub 2}: Li were used as reducing agent for the reduction of Cr{sup 6+} to Cr{sup 3+}. - Abstract: We have proposed a simple one pot synthesis of lithium-doped TiO{sub 2} nanoparticles (TiO{sub 2}:Li) via an ionic liquid-assisted hydrothermal method and theirmore » potential use as a photocatalyst for the degradation of organic dye, as well as the reduction of toxic Cr{sup 6+} to non toxic Cr{sup 3+}. The structure of TiO{sub 2}:Li nanoparticles was examined by XRD, FTIR, XPS, Raman, UV–vis, Photoluminescence spectroscopy and morphology by SEM and TEM. The incorporation of Li into anatase-phase TiO{sub 2} affected the optical properties of the resultant TiO{sub 2} nanoparticles. The photocatalytic activity of the TiO{sub 2}:Li nanoparticles was determined by degradation of trypan blue. Degradation studies showed improved photocatalytic activity of TiO{sub 2}:Li nanoparticles compared to TiO{sub 2} nanoparticles and bulk TiO{sub 2}. TiO{sub 2}:Li nanoparticles also functioned as a detoxification agent which was confirmed by the reduction of Cr{sup 6+} to Cr{sup 3+}.« less
  • Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 Degree-Sign C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn{sub 2}S{sub 4}, which shows that the ZnIn{sub 2}S{submore » 4} sample synthesized at 195 Degree-Sign C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment. - Graphical abstract: Marigold-like ZnIn{sub 2}S{sub 4} microspheres were synthesized by a fast microwave-assisted hydrothermal method at 80-195 Degree-Sign C with a very short reaction time of 10 min. The as-prepared ZnIn{sub 2}S{sub 4} sample can be used as visible light photocatalyst for degradation of organic dyes. Highlights: Black-Right-Pointing-Pointer ZnIn{sub 2}S{sub 4} microspheres were synthesized by microwave-assisted hydrothermal method. Black-Right-Pointing-Pointer The crystal structure and optical property of the products were almost the same. Black-Right-Pointing-Pointer Increment of the temperature renders high surface area due to the bubbling effect. Black-Right-Pointing-Pointer The ZnIn{sub 2}S{sub 4} synthesized at 195 Degree-Sign C shows the best visible catalytic activity for MO.« less