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Characterization of Bi-doped FAPbI3 perovskite films investigated by X-ray absorption spectroscopy
(2025-12-01)
Wechprasit, Tirapat
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Bootchanont, Atipong
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Infahsaeng, Yingyot
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Wongjom, Poramed
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Wannapaiboon, Suttipong
A thorough investigation of perovskite structures formed through doping is essential for advancing the efficiency and stability of perovskite solar cells. In this study, Bi-doped FAPbI<inf>3</inf> perovskite films with varying Bi concentrations (0.5–2%) were fabricated using a spin-coating technique on ITO glass substrates. Then the films’ phase structure, local structure, and optical characteristics were analyzed. X-ray diffraction (XRD) analysis revealed that the pristine FAPbI<inf>3</inf> film exhibited both hexagonal and cubic phases, indicating structural instability. In contrast, Bi-doped FAPbI<inf>3</inf> films predominantly displayed a cubic perovskite structure, with a notable reduction in the XRD peak intensity corresponding to the hexagonal phase. UV–Vis spectroscopy showed that the undoped FAPbI<inf>3</inf> film had an absorption edge in the visible-near infrared range, while Bi-doping caused a redshift, indicating a reduction in the optical band gap. The calculated results show that optical band gaps decrease with increasing Bi, from a value of 1.49 (pure) to 1.43 (2% Bi) eV. X-ray absorption near edge structure (XANES) analysis confirmed the oxidation states of Pb2+ and Bi3+ ions across all samples, with Bi ions replacing Pb in the local structure. Photoluminescence (PL) measurements revealed an increased PL intensity with 1% Bi doping (7 105) compared with pristine FAPbI<inf>3</inf> (4.7 105), suggesting a reduction in carrier recombination. These findings demonstrate the potential of Bi-doping to stabilize perovskite structures with improved optoelectronic properties.
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Structural and Optical Properties of Mn-Incorporated BiVO4 Nanoparticles Synthesized by Sonochemical Process
(2022-01-01)
Wechprasit, Tirapat
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Kansaard, Thanaphon
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Bootchanont, Atipong
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Pecharapa, Wisanu
In this work, Mn-incorporated BiVO<inf>4</inf> nanoparticles with different Mn contents (0–5%) were synthesized by one-step sonochemical process. Structural phase of Mn-incorporated BiVO<inf>4</inf> nanoparticles was extensively carried out by X-ray diffraction technique. The XRD results show that the structural phase of BiVO<inf>4</inf> belongs to the monoclinic principal structure while the secondary phases of MnO, Mn<inf>2</inf>O<inf>3</inf>, and Mn<inf>3</inf>O<inf>4</inf> structures are noticed in Mn-loaded samples. Chemical bondings of Mn-incorporated BiVO<inf>4</inf> nanoparticles were characterized with Raman spectroscopy. Relevant chemical bondings confirm the existence of VO<inf>4</inf>3− tetrahedron and the V–O band by Raman spectra. Diffuse reflection spectroscopy and FE-SEM were employed to examine their optical and morphological properties, respectively. The results indicate that the incorporation of Mn can induce the red-shift of optical absorption edge in visible range, which can decrease the optical band gap of BiVO<inf>4</inf>. Morphology of all samples demonstrates the difference in shape of the compounds with the incorporation of Mn contents. Oxidation number and local structure of Mn-incorporated BiVO<inf>4</inf> nanoparticles were investigated by X-ray absorption spectroscopy. XAS results demonstrate that oxidation number of all elements correspond to Mn2+/Mn3+, Bi3+, and V5+ ions. The normalized Mn K-edge XANES spectra suggest that Mn atoms would not locate at the local site of Bi or V in BiVO<inf>4</inf> crystal because the specific feature of experimental spectra are inconsistent with simulated spectra, which is corresponded to XRD results indicating the formation of Mn-based oxide structures with various oxidation states.
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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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Nonlocal XANES pre-edge feature of FeTiO3 ilmenite-type at Ti and Fe K-edge
(2020-09-01)
Phoohinkong, Weerachon
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Boonyarattanakalin, Kanokthip
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Mekprasart, Wanichaya
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Pavasupree, Sorapong
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Pecharapa, Wisanu
The pre-K-edge feature of Ti and Fe XANES of ilmenite FeTiO<inf>3</inf> were investigated. The electronic structure of FeTiO<inf>3</inf> was examined based on the partial density of electronic state distribution on both local and nonlocal atoms. A strong contribution of nonlocal metal-metal intervalence electronic states of Ti and Fe pre-K-edge was observed in X-ray absorption near-edge structure (XANES) measurement. This observation agrees well with the calculated local state density. The nonlocal excitation transitions in the pre-edge feature contribute to local pre-K-edge at both Ti and Fe. Ti pre-K-edge consists of highly hybridized Ti-3d(t<inf>2g</inf>) with a small part of dipole-allowed 4p and a small 4s density transition state feature which is predominated by nonlocal of Fe-3d mixed with 4p state delocalized via O-2p as the main component peak. The peak feature at Ti-3d(e<inf>g</inf>) energy state is assigned to hybridization of Ti-3d(e<inf>g</inf>) and Ti-4p state contributed with nonlocal of the hybridized Fe-sp and the Ti-pd state. Fe pre-K-edge shows two main prominent transition peaks of hybridized Fe-pd state and the delocalized local Fe-sp with nonlocal Ti-3d(t<inf>2g</inf>) and 4p mixing states centered at 7112.38 and 7116.48 eV, respectively. The local and nonlocal excited transition energy states and density of both Ti pre-K-edge and Fe pre-K-edge features are corresponded with each other through the O-2p state transition pathway.
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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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X-ray absorption spectroscopy analysis and magnetic properties of M-doped TiO2 nanoparticles (M=Co, Mn, Ni and Zn) prepared by co-precipitation method
(2017-08-01)
Wattanawikkam, Chakkaphan
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Pecharapa, Wisanu
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Ishihara, Keiichi N.
M-doped TiO<inf>2</inf> nanoparticles (M=Co, Mn, Ni and Zn) were synthesized by co-precipitation method combined with annealing at 500 °C for 2 h. X-ray diffraction (XRD) was used to identify their structural phases. X-ray absorption near edge structure (XANES) was conducted to probe the chemical state and crystal atomic structure of prepared samples. Magnetic properties of all samples were characterized by vibrating sample magnetrometer (VSM). The XRD analyses reveal that all samples crystallize in anatase tetragonal structure with no additional peaks. The XANES spectra exhibit triple pre-edge fingerprint of Ti4+ of oxidation state with six-fold octahedral coordinate structure. Co-, Ni- and Zn- K-edge results indicate that the Co, Ni and Zn ions in M-doped TiO<inf>2</inf> are in 2+ formal oxidation state. Meanwhile, Mn-doped TiO<inf>2</inf> sample contains the different oxidation states of 3+ and 4+. The amount of each oxidation state is confirmed by using linear combination fitting method. The magnetic measurement illustrates the paramagnetic behavior for Co-, Mn- and Ni- doped samples that strongly depend on the doping content and no hysteresis loop is observed in undoped and Zn-doped samples.
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Structural, optical and magnetic properties of diluted magnetic perovskite ZnTiO3 doped with Co and Mn prepared by sonochemical method
(2017-01-01)
Wattanawikkam, Chakkaphan
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Phoohinkong, Weerachon
;
Pecharapa, Wisanu
We employed a sonochemical method to fabricate transition metal ion doped perovskite ZnTiO<inf>3</inf> (M-ZnTiO<inf>3</inf>) nanoparticles, including individual Co and Mn ions. The Zn:Ti was mixed in molar ratio of 1:1 to obtain starting precursor for ZnTiO<inf>3</inf>. The different concentrations of Co (5-10 mol%) and Mn (3-7 mol%) were doped in ZnTiO<inf>3</inf>, then the mixing solution were irradiated in high frequency ultrasound of a sonometer (20 kHz, 750 W) at room temperature to obtain the as-prepared samples. The final products were calcined at 800°C for 3 h to improve the crystallinity. We confirmed formation structures of M-ZnTiO<inf>3</inf> nanoparticles by X-ray diffraction (XRD), and used X-ray absorption near edge spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS) technique to investigate the crystal structure and valence states of the sample. Meanwhile, we studied their optical properties by diffuse reflectance spectroscopy, and evaluated magnetic properties of the samples at room temperature by vibrating sample magnetometer (VSM). Magnetization measurements revealed the paramagnetic behavior for Co-ZnTiO<inf>3</inf> and weak ferromagnetic behavior for Mn-ZnTiO<inf>3</inf>. We also investigated and discussed the effect of metal ion doping concentration on the structural, optical and magnetic properties.
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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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