Abstract
In this study, pure, Nickel, and Cobalt-doped ZnO nanofibers are synthesized successfully by an electrospinning technique. The Ni2+ and Co2+ ions doping effect on the structural, morphological, optical, and magnetic behavior of ZnO nanofibers are investigated by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), UV-vis diffuse reflectance spectrophotometer (DRS), Vibrating sample magnetometer (VSM). The XRD analysis results reveal that all samples have hexagonal wurtzite structures. Ni and Co atoms have been successfully incorporated in tetrahedral sites and no secondary phases were detected. DRS spectra indicates that the band gap value varied from 3.18 eV for ZnO to 3.20 eV for ZnO: Ni and 2.82 eV for ZnO: Co. The FTIR spectra exhibit the characteristics absorbance peaks at 438 cm−1, 432 cm −1, and 437 cm−1 for pure, Ni-doped ZnO, and Co-doped, respectively. The VSM results show all sample’s ferromagnetic behavior at room temperature.
Introduction
Zinc oxide (ZnO) is an n-type semiconductor with a direct energy band gap (3.37 eV at room temperature), a large exciton binding energy (60 meV), and excellent thermal and chemical stability1. These properties of ZnO provide it numerous potential applications in photoelectronic devices2,3,4, sensors5, photocatalysis6,7. Extreme transparency, nontoxicity, biocompatibility, and high absorption spectral range help ZnO to be applied as biosensors, bio-imaging material, photocatalysts in the environment for water and air cleaning, and as a transparent electrode in solar cells8,9,10,11.
Among the ZnO nanostructure, ZnO nanofibers have attracted considerable attention in the last decade due to their large aspect ratio, high electron mobility, and electrical and optical anisotropy12. The properties of ZnO strongly depend on the size of the material. For example, for larger sizes the recombination rate of photo-induced electron-hole pairs is higher, resulting in poor photo-catalytic activity12.
ZnO is a versatile material for doping different transition metals among other metal oxide. Doping of transition metal ions in ZnO nanofibers can effectively improve the optical, dielectric, and magnetic properties. In addition, room-temperature ferromagnetic behavior is obtained by doping with transition metal ions into ZnO nanostructures13.
The efficiency of dopant elements depends on the electronegativity and radius Difference between the dopant ion and Zn ion. Among the transition dopant elements, Ni have ionic radii of 0.69Ao and 0.72Ao, Close to the ionic radius of zinc (0.74Ao). They can easily incorporate into zinc lattice sites without change in the crystal structure of ZnO14,15. Doping Ni and Co in ZnO nanofibers produces more charge carriers that improve their conductivity.
The incorporation of Co2+ ions into the ZnO lattice includes not only the replacement of ZnO ions on regular Zn sites but also positioning of Co on non-regular (such as interstitial) sites. Therefore, magnetic properties of Co doped ZnO nanosamples can be due to the concentration and distribution of Co2+ ions and the concentration of intrinsic defects. Furthermore, Co2+ ions in the half-filled 3d shell have five spins, which normally provide a maximum dipole moment value in the structure. Therefore, Co doping in ZnO is assumed to modify the properties of the spin-based devices through enhanced magnetic properties16,17.
Recently, there have been some reports about the effect of doping the transition metal (Ni2+, Co2+,) on the properties of ZnO nanofibers18,19. Younus Ali et al. investigated the effect of Ni doping on the structure, morphology, and optotransport properties of spray-pyrolised ZnO nanofiber. Their study exhibits red shifting in band gap energy and decreases remarkably resistivity with Ni20. In another study, Srinivas et al. reported the room-temperature ferromagnetism behavior of nickel-doped ZnO nanoparticles21.
Eppakayala et al. investigated the effect of different concentration of Ni to the absorption and structural properties of ZnO, indicating not only enhancing the electron-hole pair separation by decreasing the band gap but also decreasing the average grain size22.
The influence of Co2+ ions doping on the structural, morphological, optical, and magnetic properties of ZnO nanoparticles was shown by Pazhanivelu et al. They revealed that increasing dopant concentration decreases lattice parameters, unit cell volume, bond length, average crystallite size, and band gap of ZnO nanoparticles23.
Shatnawi et al. synthesized undoped and co-doped ZnO nanoparticles observed ferromagnetic behavior with relatively small coercive fields at room temperature and also found a strong correlation between the magnetic and optical behavior of the Co-doped ZnO nanoparticles24.
Among the different methods for producing nanofibers, Electrospinning is a simple and low-cost method for preparing continuous nanofibers with uniform diameters and various compositions25. Many papers report the preparation of electrospun ZnO nanofibers obtained from ZnO precursor solutions mixed with polyvinyl alcohol (PVA)26, polyvinylpyrrolidone (PVP)27, or polyvinyl acetate (PVAc)28.
In this study, pure, nickel, and cobalt-doped ZnO nanofibers are synthesized by electrospinning technique, and the doping effect of Nickel and Cobalt on the structural, optical, and magnetic properties of ZnO nanofibers is studied at room temperature.
Experimental
Materials
Polyvinyl alcohol (PVA; Mw = 150 000) and Zinc acetate dehydrate. (Zn (CH3COO)2·2H2O), Nickel(II) acetate tetrahydrate (Ni(CH3CO2)2·4 H2O), and cobalt acetate the tetrahydrate Co(CH3CO2)2·4 H2O as the precursors, were obtained from Sigma-Aldrich. Electrospinning was carried out using an Electroris electrospinning unit (eSpinner NF CO-N/VI, Iran; https://www.anstco.com) with a high voltage of 1–35 kV. Drying, annealing, and carbonization were carried out using a muffle furnace (FM8P, Iran; https://farazmaco.com).
Preparation of ZnO nanofibers
In a typical procedure, the ZnO nanofibers was synthesized using an electrospinning technique. First, 1 g PVA was dissolved in 8 mL of distilled water. The solution was stirred continuously using a magnetic stirrer (Delta model HM-101) at room temperature for 1 h. 0.6 g Zn (CH3COO)2·2H2O was dissolved in 2 ml deionized water for 20 min. Then the two solutions were mixed for 1 h. The as-prepared solution was transferred into a plastic syringe. The electrospinning procedure was performed at an applied voltage of 18 kV, a solution flow rate of 0.4 mLh−1, and a needle-to-collector distance of 18 cm. Finally, the collected fibers were dried at 60ºC for 15 min, then annealed at 500ºC for 3 h in air.
Preparation of ZnO: Ni and ZnO: Co nanofibers
The Co-doped ZnO nanofibers with dopant concentrations of 5 mol% were synthesized by sol-gel based on an electrospinning process. In a typical experiment, 0.8 g of PVA was added to 8 mL of distilled water with vigorous stirring for 1 h. A 0.47 g of zinc acetate (Zn (CH3 COO)2) and nickel acetate Ni(OCOCH3)2·4H2O were dissolved in 2 ml of deionized water for 20 min. Then, the solution was added to the PVA solution with vigorous stirring for 1 h to form a viscous gel. The solution was then electrospun at applied high voltage (18 kV) and needle to collector distance (18 cm), and flow rate 0.5 ml/h. The collected electrospun nanofibers were dried at 125 ◦C for 6 h. The dried electrospun precursors were then annealed in a furnace at 500 ◦C for 2 h in air. The same procedure was used to prepare ZnO: Co using 0.47 and 0.03 g of Zn (CH3COO)2 and Co(CH3CO2)2·4H2O as a source of ZnO and Co, respectively. The ZnO nanofiber preparation process is shown schematically in Fig. 1. Also, related image can be seen in the supplementary file as Fig. 1.
Fig. 1
figure 1
Schematic of the preparation process of samples.
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Characterization
Scanning electron microscopy (FE-SEM; Stereo Scan 360) was performed to study the morphologies of the nanofibers. Structural characterization of ZnO, ZnO: Ni, and ZnO: Co nanofibers were examined by X-ray diffraction (Philips X’Pert X-ray diffractometer using CuKa radiation (wavelength = 1.54056 Å) at 40 kV and 30 mA). The chemical structure of the nanofibers was performed on Fourier transform infrared spectrometer (Varian-3600 FT-IR spectrometer) with KBr crystals in the infrared region between 400 and 4000 cm−1. The optical absorption behavior of the fibers was studied by UV-vis diffuse reflectance spectrophotometer (UV-DRS, SCINCO: S-4100). The magnetic properties of samples were investigated by VSM analysis vibrating sample magnetometer (Magnetic Daghigh Kavir: MDKB measurements).
Results and discussion
The surface morphologies of the pure and doped ZnO precursor nanofibers prepared by electrospinning were observed by SEM (Fig. 2a, c & e). The nanofibers have a random orientation with a smooth and uniform surface. The diameter of the Pure and Ni, Co-doped ZnO precursor nanofibers were determined as 470, 417, and 426 nm, respectively. Figure 2(b, d & f) shows SEM image of calcined ZnO Ni-doped and Co-doped ZnO nanofibers at 500ºC in air. These nanofibers exhibit typical nanofiber network structure with 180.7, 133, 128 nm in diameter. After calcination at 500 ◦C, the average diameters of all the nanofibers shrank drastically. The shrinkage in fibers diameter is due to the removal of PVA from fibers and the conversion of metal salts into metal oxides. In addition, an image analyzing software (Digimizer) was used to get histogram of the diameter distributions of fibers. Distribution of the fiber diameter shown in Fig. 3.
Fig. 2
figure 2
SEM images of the ZnO nanofibers. (a) As-spun undoped ZnO precursor nanofibers; (b)undoped after calcination; (c) Ni-doped ZnO precursor nanofibers; and (d) Ni-doped ZnO nanofibers, (e) Co-doped ZnO precursor nanofibers; and (f) Co-doped ZnO nanofibers atfer calcinations at 500 c for 2h.
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Fig. 3
figure 3
diameter size distribution of fibers, (a) ZnO, (b) Ni-doped ZnO, and (c) Co-doped ZnO.
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XRD analysis
The crystalline structure of pure and doped ZnO nanofibers was investigated by X-ray diffraction analysis. Figure 4a shows the XRD patterns of ZnO, ZnO: Co, and ZnO: Ni nanofibers. The XRD patterns confirm the hexagonal structure of the ZnO lattice (space group P63mc, JCPDS No. 36–1451) with multiple peaks along (100), (002), (101), (102), (110), (103), (201) and (004) planes29,30. No additional peaks connected with the presence of such compounds as Co, Ni, NiO, and Co3O4 were observed in Co, Ni-doped ZnO nanofibers. In all XRD patterns, the (002) and (101) peaks were dominant in which (101) plane intensity is higher than the other planes. In comparison to pure ZnO, high-intensity peaks of Ni-ZnO in XRD confirm the micro-crystalline nature of Ni: ZnO nanofibers31.
In addition, the (002) peak position was shifted towards a higher angle for doped samples (Fig. 4b). The higher 2θ exhibits lattice contraction due to the ionic radii of Co and Ni ions being smaller than Zn ions. This result maybe attributes the incorporation of Ni and Co ions into the ZnO lattice.
The crystal structures were obtained via Rietveld refinement of the X-ray diffraction profiles with the material analysis using diffraction (MAUD) program (Fig. 5). The lattice parameters and the crystallographic position of each element of ZnO nanofibers are shown in Tables 1 and 2, respectively32,33. The data indicated that doping zinc oxide with Na and Co does not substantially affect the lattice parameters, which is expected due to the small difference between the ionic radius of the Zn (0.72 Å) and Co (0.745 Å) and Ni(0.69 Å).
The slightly decrease of lattice parameter values of pure ZnO (Table 1) by doping is probably due to the grain growth of ZnO being suppressed by the Co and Ni ions. This could be due to the Co and Ni ions can easily enter the regular lattice site of ZnO, due to a smaller ionic radius as compared with Zn. In addition, some of the Zn2+ replaced by Co2+ and Ni2+ ions, as a result decreasing the grain size and increasing oxygen the oxygen deficiency30,34.
The average crystallite size was determined using MAUD for undoped and Ni and Co-doped ZnO nanofibers are approximately 44.93, 37.77 and 53.89 nm, respectively. The crystallite size decreases with the addition of Ni. This is due to the dopant-induced resultant drag forces against the crystallite size growth, which leads to a smaller crystallite size. The crystallite size increases with the addition of Co. This increase may be due to nucleation that enhances the grain growth of Co-doped ZnO nanofibers.
Fig. 4
figure 4
The X-ray diffraction patterns of different samples.
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Fig. 5
figure 5
Experimental and refined patterns from Rietveld refinement for the ZnO, ZnO: Ni, and ZnO: Co nanofibers.
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Table 1 Lattice parameters of the sample and goodness of fit.
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Table 2 Crystallographic positions of the elements Zn and O in ZnO, ZnO: Ni, and ZnO: Co.
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Table 3 Magnetic properties of Ni and Co doped ZnO nanostructure reported in literature.
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FTIR analysis
The chemical composition, information about chemical bonding, and vibration position of the material were investigated by FTIR spectroscopy. The presence and position of the absorption bands depend on the chemical composition, crystal structure, and morphology. The FTIR spectra of pure and doped (Co and Ni) ZnO nanofibers are shown in Fig. 6.
The peaks in the ranges of 430 to 550 cm−1, correspond to Zn–O stretching vibrational Modes35. The change in the bond lengths of the Zn–O lattice by the replacement of Ni and Co ions instead of Zn ions leads to a shift of the vibration frequency of Zn–O to a frequency lower than 438 cm−1corresponding to undoped ZnO. This confirms the incorporation of Ni2+ and Co2+ ions as a substitute for Zn2+ ions in the ZnO structure36.
The peaks around 1630 cm−1 and the peak at 3420 cm−1 are assigned to the O–H bending and stretching frequency of water molecules, respectively. The peak around 1460 cm−1 corresponds to C-O stretching37.
Similar spectra were obtained for Co-doped and pure ZnO nanofibers. The existence of shift in the frequencies as Ni2+ dopant may be due to the difference in the bond length as Zn2+ with higher ionic radius is replaced by Ni2+ and Co2+ with different ionic radius, which confirms the incorporation of Co2+ and Ni2+in the ZnO lattice38.
Fig. 6
figure 6
FTIR spectra of ZnO and Co, Ni-doped ZnO.
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Optical properties
Figure 7 shows the DRS spectra of undoped and doped ZnO nanofibers. The absorption band edge for ZnO nanofibers was observed at ~ 370 nm. Compared with undoped ZnO, the Co doped ZnO nanofibers show red-shift absorption band edge of 405 nm and narrowed band gap of 2.82 eV. This band gap narrowing due to the formation of various optically active sub-levels through the bandgap of ZnO. The absorption spectrum of Ni-doped ZnO nanofibers shows that the absorption peak value is slightly shifted towards the lower wavelength (blue shift).
Moreover, The Co-doped ZnO nanofibers show the peaks at 568, 610, and 659 nm. These peaks assigned to the d–d crystal-field transitions 4A2 (F) → 2A1 (G), 4A2 (F) → 4T1 (P), and 4A2 (F) → 2T1 (G) in high spin states (S = 3/2). the appearance of these transitions indicate that the doped Co2+ ions are under a tetrahedral crystal field, and most of Co ions are in high-spin states (S = 3/2). The Zn+2 sites in the wurtzite crystal structure have a tetrahedral coordination. Therefore Co2+ ions were substituted for Zn2+ sites in the ZnO lattice39,40.
The optical band gap was determined by the first derivative method of absorption data with respect to the photon energy (Fig. 8). The band gap value varied from 3.18 eV for ZnO to 3.20 eV for ZnO: Ni and 2.82 eV for ZnO: Co. The variation of the band gap shows the incorporation of Co and Ni in the ZnO matrix.
The shift of the absorption peak value is due to the size effect, where the crystallite size decreases on Ni ion doping and increase on Co ion doping. In addition, The red-shift in band gap with Co doping can be attributed to the sp-d exchange interaction between the ZnO band electrons and the localized d-electrons (moments) of doped Co ions which raise the O 3p valence band and lower the Zn 4s conduction band41,42.
Fig. 7
figure 7
The absorbance spectra of undoped and doped ZnO nanofibers.
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Fig. 8
figure 8
The first derivative of the absorbance data versus energy for undoped and doped ZnO nanofibers.
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Magnetic properties
The magnetic properties of nanofibers were examined by the VSM analysis. Figure 9 shows the magnetization versus magnetic field (M–H) plots of all the samples. The first derivative of the magnetization (M) with respect to H for the sample is also plotted in Fig. 10. All samples show ferromagnetic behavior at room temperature. It’s evident from the magnetic characterization that Co and Ni-doped ZnO nanofiber shows a higher degree of magnetization than pure ZnO. The ferromagnetic behavior was increased for Ni and Co-doped ZnO. The magnetic properties of a system depend on the concentration and distribution of the transition metal ions, type, and concentration of defects, n-type doping, and p-type doping43.
The ferromagnetism behavior observed in Co, Ni-doped zinc oxides was usually attributed to the formation of some intrinsic point defects such as zinc vacancy (Vzn ), zinc interstitial (Zn i ), oxygen antisite (O zn ), oxygen interstitial (Oi ) as well as due to the presence of magnetic ions (like Ni, Co) replacing non-magnetic element (Zn, ) within the crystal lattice. Magnetic cations, carriers, and defects make up bound magnetic polarons (BMPs). According to the (BMP) model, bound electrons (holes) in the defect states can couple with transition metal ions and cause the ferromagnetic regions to overlap, giving rise to long-range ferromagnetism ordering15,44,45.
The BMP concentration cannot fully account for the observed high magnetic moment in the doped ZnO nanofibers. Further, some isolated Ni+2(Co+2) ions might interact by antiferromagnetic interaction41. The existence of strongly antiferromagnetic interactions between Ni+2(Co+2) ions decreases the saturation magnetic moment per atom46.
The remanent magnetization (Mr), susceptibility (χ), and magnetic coercivity (Hc) of pure ZnO and doped ZnO nanofibers compared with the results of the other works [Table 3].
Fig. 9
figure 9
Magnetization vs. magnetic field curve measured at room temperature of pure and Co, Ni-doped ZnO.
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Fig. 10
figure 10
Magnetization vs. magnetic field curve, and the first derivative of M with respect to H for (a) ZnO, (b) ZnO: Ni (c) ZnO: Co.
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Conclusion
The electrospinning technique was successfully applied to prepare undoped and doped ZnO nanofibers. Morphological characterization based on the recorded SEM images of undoped and doped ZnO nanofibers, showed that the obtained morphology can be classified as nanofiber structures, and the shrinkage in fibers diameter is due to the removal of PVA from the fibers structure. XRD analysis confirms that the samples are highly crystalline with hexagonal wurtzite structure, without any secondary phases. The band gap values of undoped and doped ZnO nanofibers with Ni (5%) and Co (5%) were estimated by to be 3.18, 3.20 and 2.82 eV, respectively, affected by the size effect. The magnetic properties of nanofibers show ferromagnetic nature of the nanofibers.
Data availability
The authors declare that the data supporting the findings of this study are available within the paper and its supplementary information file.
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Authors and Affiliations
Department of physics, Faculty of science, University of Guilan, Namjoo Ave, PoBox, Rasht, 41335- 1914, Iran
Fatemeh Heydari Vieii, Roya Shokrani Havigh & Hossein Mahmoudi Chenari
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Fatemeh Heydari Vieii
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2. Roya Shokrani Havigh
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3. Hossein Mahmoudi Chenari
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Contributions
Fatemeh Heydari Vieii prepared nanofibers. Roya Shokrani Havigh contributed to writing part—original draft, testing measurements. Hossein Mahmoudi Chenari contributed in Review and editing, Supervision, Project administration.
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Correspondence to Hossein Mahmoudi Chenari.
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Vieii, F.H., Havigh, R.S. & Chenari, H.M. Electrospun preparation of nickel and Cobalt-doped ZnO fibers: study on the physical properties. Sci Rep 15, 10898 (2025). https://doi.org/10.1038/s41598-025-95443-7
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Received:18 December 2024
Accepted:20 March 2025
Published:29 March 2025
DOI:https://doi.org/10.1038/s41598-025-95443-7
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Keywords
ZnO
Doping
Nanofibers
Physical properties