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Characterization, X-ray absorption spectroscopic analysis and photocatalytic activity of Co/Zn co-doped TiO2 nanoparticles synthesized by one-step sonochemical process
(2021-10-01)
Mekprasart, Wanichaya
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Pavasupree, Sorapong
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Jayasankar, C. K.
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Ravuri, Balaji Rao
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Wattanawikkam, Chakkaphan
A novel one-step preparation of sonochemical method was applied to synthesize Co/Zn co-doped TiO<inf>2</inf> nanoparticles using a sonicator of 750 W, 20 kHz for 30 min at room temperature. The formation of the anatase TiO<inf>2</inf> phase for all as-prepared samples was observed from XRD results with a crystalline size in nanoscale. The use of ultrasound allowed for the successful doping of both Co and Zn into the TiO<inf>2</inf> lattice, which was confirmed by Synchrotron light including X-ray near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS) spectroscopy. Ti K-edge, Co K-edge, and Zn K-edge XANES spectra exhibited the dominating +4, +2, and +2 valence state of Ti, Co, and Zn in as-prepared samples, respectively. A detailed XANES and EXAFS data analysis give strong evidence that the Co/Zn dopants partially replace the Ti atom of the TiO<inf>2</inf> host. The Co/Zn co-doping extends the light absorption of the host to the visible region and restricts the e+/h+ recombination. The photocatalytic activity of samples was tested for degradation of Rhodamine B dye solution under visible light irradiation. The as-synthesized of the co-doped catalyst was presented as highly efficient, with 2.5 and 5 times dye degradation compared with single-doped and bare TiO<inf>2</inf>.
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Structural studies and photocatalytic properties of Mn and Zn co-doping on TiO2 prepared by single step sonochemical method
(2020-06-01)
Wattanawikkam, Chakkaphan
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Pecharapa, Wisanu
Titanium dioxide nanoparticles dual doped with zinc and manganese were prepared by the single step of sonochemical method using the sonicator with 20 kHz and 750 W for 30 min. Phase structure analysis results showed that the pure anatase phase was detected for all prepared samples. TEM analysis reveals the nanosized structure with uniformity of nanoparticles. The calculated bandgap energies change to be below the typical band gap energy of bare TiO<inf>2</inf> and single doped sample suggesting high ability to harvest visible light. X-ray absorption spectroscopy was conducted to investigate the electronics structure and to study the local structure of prepared samples. XANES results confirmed the existence of Ti4+ ions in all prepared samples with anatase crystal structure. EXAFS analysis indicates the Ti4+ site was substituted by Mn and Zn dopant ions. The photocatalytic performance was evaluated by degradation of Rhodamine B dye solution under visible light irradiation. The results revealed that the dually Mn–Zn doped TiO<inf>2</inf> sample exhibited excellent photocatalytic activity comparing to single doped and pure TiO<inf>2</inf>. The complete degradation of dye was achieved at optimum condition of 1 mol%-Zn and 2 mol%-Mn molar ratio. The highest photodegradation rate constant was found to be 0.0238 min−1, which is 10 times greater than pure-TiO<inf>2</inf> samples.
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X-ray absorption spectroscopy analysis and photocatalytic behavior of ZnTiO3 nanoparticles doped with Co and Mn synthesized by sonochemical method
(2019-04-30)
Wattanawikkam, Chakkaphan
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Kansa-ard, Thanaphon
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Pecharapa, Wisanu
ZnTiO<inf>3</inf> (ZTO) as a perovskite structure doped with Co and Mn were fabricated by sonochemical process. Structural phase, chemical and local atomic structure and photocatalytic activity of the synthesized samples were characterized, by X-ray diffraction, by X-ray absorption spectroscopy and Rhodamine B (RhB) dye degradation. The XRD results revealed that the mixing phases of cubic and hexagonal zinc titanate phases were found in all samples. The X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure technique (EXAFS) have been used to identify the crystal and atomic local structure of prepared samples. The Fourier transform EXAFS results of these prepared samples agreed well with the model of Co and Mn substituting at the B-site of ABO<inf>3</inf> structure together with small cluster of CoO and Mn<inf>2</inf>O<inf>3</inf> cluster. The photocatalytic activity for rhodamine b dye degradation under visible light irradiation exhibited that the doped samples had the superior degradation compared to bare-ZTO sample. The results suggest that the incorporation of transition metal ions of Co and Mn dopants is an effective way to improve the catalytic efficiency of perovskite ZTO structure. The effect of different dopant ions and dopant concentration on the structural, chemical, optical and photocatalytic activity are discussed.
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ACTIVE-ILMENITE SURFACE STRUCTURE INFLUENCE ON ACID-ASSISTED BALL MILLING
(2018-12-01)
Phoohinkong, Weerachon
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Pavasupree, Sorapong
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Boonyarattanakalin, Kanokthip
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Mekprasart, Wanichaya
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Pecharapa, Wisanu
Active-ilmenite powder derived from natural ilmenite sand was prepared by the ball milling process with acid-solution and Deionized (DI) water. Morphology and particle size of active-ilmenite product in acid/DI-assisted ball milling process were monitored by field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). Surface atomic component and chemical bonding were investigated by X-ray photoelectron spectroscopy (XPS). Meanwhile, bulk chemical oxidation and fine structure of active-ilmenite were studied by X-ray absorption near edge structure (XANES) and extended X-ray absorption ne-structure spectroscopy (EXAFS) to confirm the oxidation state and local active species structure at surface. Active-ilmenite by acid-assisted ball milling process is a distinctive method for the preparation of active-ilmenite product with high active surface. Moreover, the distortion of TiO <inf>6</inf> and FeO <inf>6</inf> octahedral cluster on the sample surface was detected in all milled samples with acid-assisted ball milling process. The presence of Fe 2+ , Fe 3+ ions and miniature sulfate was also detected on the sample surface by milled product with acid-assisted method.
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The disordered cation distribution studies of nanosized zinc ferrite powders by synchrotron X-ray absorption spectroscopy
(2016-04-26)
Tangcharoen, Thanit
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Klysubun, Wantana
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Kongmark, Chanapa
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Pecharapa, Wisanu
The non-equilibrium site occupancy of zinc (Zn2+) and ferric (Fe3+) ions in dissimilar nanosized zinc ferrites (ZnFe2O4)powders obtained from the different milling time (0 to 24 h) of the as-combusted powders was investigated through Zn and Fe K-edge X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectra. Compared with the bulk specimen of zinc ferrite, both XANES and EXAFS spectra of nanosized zinc ferrite powders clearly exhibit the large Zn2+ ions translocation from the tetrahedral (A) sites to the octahedral (B) sites leading to the movement of many Fe3+ ions in the opposite direction without the variation in the long-range structural order.
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Synchrotron X-ray absorption spectroscopy study of disordered cation distribution of nanosized zinc ferrite powders
(2016-01-01)
Tangcharoen, Thanit
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Kongmark, Chanapa
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Klysubun, Wantana
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Pecharapa, Wisanu
The zinc ferrite (ZnFe<inf>2</inf>O<inf>4</inf>) powders of various nanoparticle sizes were synthesised at different milling times (0 to 24 h) of the as-combusted powders. The non-equilibrium site occupancy of zinc (Zn2+) and ferric (Fe3+) ions was investigated through Zn and Fe K-edge X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectra. The XRD and SEM strongly confirm the particle size of these ferrites decreasing with the increasing milling time. Compared with the bulk specimen of zinc ferrite, both XANES and EXAFS spectra of zinc ferrite powders clearly exhibit the large translocation of Zn2+ ions from the tetrahedral (A) sites to the octahedral (B) sites and the opposite translocation of some of Fe3+ ions without affecting the long-range structural order. Moreover, the curve-fitting analysis of Zn and Fe K-edge EXAFS spectra indicates that the degree of inversion increases as the particle size decreases resulting in significant differences in the magnetic behaviours.
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Synchrotron X-ray absorption spectroscopy study of the local atomic structures and cation ordering in perovskite- and spinel-type zinc stannate synthesized by co-precipitation method
(2015-12-15)
Tangcharoen, Thanit
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Kongmark, Chanapa
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Pecharapa, Wisanu
Zinc stannate nanocrystalline powders with two different crystal structures were synthesized from two different initial Zn2+/Sn4+ ratios by a simple co-precipitation method. X-ray diffraction (XRD), X-ray absorption near edge structure (XANES), and extended X-ray absorption fine structure (EXAFS) techniques were used to investigate crystal structure, oxidation, and cation ordering of the after-calcined powders. XRD patterns clearly showed that the ZnSnO<inf>3</inf> perovskite phase was obtained using an equal initial Zn2+/Sn4+ ratio of 1:1, while a double Zn2+ excess sample (2:1) produced the pure Zn<inf>2</inf>SnO<inf>4</inf> spinel phase. The chemical shifts in Zn K- and Sn L3-edge XANES spectra supported that only Zn2+ and Sn4+ ions existed in these stannate samples. Moreover, the theoretical simulation of the Zn K-edge EXAFS experimental data also indicated a change in the cation ordering from orthorhombic, for perovskite ZnSnO<inf>3</inf>, to cubic for spinel Zn<inf>2</inf>SnO<inf>4</inf>. This is the first time that the local atomic structural characterization of zinc stannate powders derived from EXAFS analysis has been presented.
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A comparison of cation distribution and valence state in spinel crystal structure of zinc and nickel ferrites using the synchrotron X-ray absorption spectroscopy (XAS) analysis
(2014-07-24)
Tangcharoen, Thanit
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Klysubun, Wantana
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Ruangphanit, Anucha
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Pecharapa, Wisanu
In this work, the physical structure, magnetism and local structure of zinc and nickel ferrites (ZnFe<inf>2</inf>O<inf>4</inf> and NiFe<inf>2</inf>O <inf>4</inf>) synthesized by typical sol-gel combustion method, were investigated by X-ray diffraction (XRD), vibrating sample magnetometer (VSM), X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). The formation of the single phase cubic spinel crystal structure and the different values of crystallite size (D), interplanar distance (d) and lattice constant (a) for all ferrite samples were evaluated by the XRD data. The VSM measurement provides the characteristic magnetic hysteresis loop (M-H) for each sample which was found to be significantly different from each other. The chemical shifts in Zn, Ni and Fe K-edges XANES spectra indicate the existence of Zn2+, Ni2+ and Fe3+ ions in these ferrites. The EXAFS spectra analyses applied to track Zn, Ni and Fe cation distribution indicate the distinct character of spinel crystal structure of both ferrites. The results exhibit that zinc ferrite is a normal spinel, while the nickel ferrite is an inverse spinel. Moreover, these EXAFS spectra analyses reveal that the distances between metal ion (Zn2+ or Ni2+) to central oxygen ion and to Fe3+ ions in the opposite lattice site for each ferrite sample are unequal which highly affect its magnetism. The overall simulated results are one of the important evidence encouraging the explanation on the paramagnetism for ZnFe<inf>2</inf>O<inf>4</inf> and the ferrimagnetism for NiFe<inf>2</inf>O<inf>4</inf>. © 2014 Taylor & Francis Group, LLC.
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Synchrotron X-ray absorption spectroscopy and magnetic characteristics studies of metal ferrites (metal = Ni, Mn, Cu) synthesized by sol-gel auto-combustion method
(2014-01-01)
Tangcharoen, Thanit
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Klysubun, Wantana
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Kongmark, Chanapa
;
Pecharapa, Wisanu
In this work, the metal ferrites MFe<inf>2</inf>O<inf>4</inf> (M = Ni, Mn, Cu) were synthesized from metal nitrate precursors by the sol-gel auto-combustion method using diethanolamine (DEA) as a potential fuel. The crystal structures of these ferrite powders were characterized by X-ray diffraction (XRD) technique confirming the complete formation of the single-phase cubic spinel crystal structure. The ferrimagnetism characteristic and the difference of the magnetic properties such as saturation magnetization (M<inf>s</inf>), remanent magnetization (M<inf>r</inf>), and coercivity (H <inf>c</inf>) for each after-calcined ferrite sample were scrutinized through the ferrimagnetic hysteresis loop (M-H) obtained from the vibrating sample magnetometer (VSM) measurement. Moreover, the cation distribution and valence state of these ferrites were investigated by the Ni, Mn, Cu, and Fe K-edge X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectra using the synchrotron radiation light source. From the XAS results, the analyses of both XANES and EXAFS spectra show the existence of accurate oxidation state for transition metal ions and the interionic distance to the nearest neighbors in the spinel crystal structure. In particular, the curve-fitting analysis of Ni, Mn, Cu, and Fe K-edge EXAFS spectra indicates that the degree of inversion in these metal ferrites is entirely different and found to be 0.2 for MnFe<inf>2</inf>O<inf>4</inf>, 0.8 for CuFe<inf>2</inf>O <inf>4</inf>, and 1.0 for NiFe<inf>2</inf>O<inf>4</inf>, which are the important information for understanding their effects on relevant magnetic properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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