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Characterization of multifunctional nanocomposites assembled from Ag-decorated Fe3O4 and Eu-doped Y2O3

Abstract

Multifunctional nanocomposites are attracting increasing interest for biomedical applications. Herein, we report the characterization of trifunctional Fe3O4–Ag@Y2O3:Eu3+ nanocomposites with surface-enhanced Raman scattering (SERS), magnetic, and fluorescence properties. Fe3O4–Ag@Y2O3:Eu3+ nanocomposites were prepared using a high-energy ball milling method. The XRD pattern of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites shows the phases of Fe3O4–Ag and Y2O3:Eu3+, implying successful conjugation of Fe3O4–Ag and Y2O3:Eu3+. Additionally, the saturation magnetization of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites was less than those of Fe3O4 and Fe3O4-Ag nanoparticles; however, it was strong enough for effective magnetic separation. The photoluminescence spectra show a strong visible red emission at 610 nm (5D0 → 7F2) at the excitation wavelength of 250 nm. Furthermore, the Fe3O4–Ag@Y2O3:Eu3+ nanocomposite substrate exhibited stronger SERS signals than the aluminum foil substrate. Therefore, the multifunctional nanocomposites Fe3O4–Ag@Y2O3:Eu3+ may be useful in biomedical systems, such as biological targeting separation, multiplex detection, and bioimaging.

Introduction

Multifunctional nanomaterials have attracted interest for their potential applications in biomedical systems including drug delivery, biochemical targeting separation, biological labeling, and multiplex detection [1,2,3,4,5]. In recent years, many studies have reported magnetic fluorescence or surface-enhanced Raman scattering (SERS)-fluorescence materials.

Fluorescence-based materials have been widely used for diagnosis, monitoring, and therapeutic imaging because of their ease of detection and wide encoding process [6,7,8]. Recently, rare-earth-doped fluorescence materials have attracted considerable attention owing to their high quantum yield, narrow linewidth, negligible toxicity, and photostability [9, 10]. Among the various rare-earth doped fluorescent materials, europium ion (Eu3+)-doped yttrium oxide (Y2O3) is a widely used red-emitting phosphor with high quantum efficiency, low phonon energy, and high thermal stability [11,12,13].

Iron oxide (Fe3O4) nanoparticles (NPs) are candidates for multifunctional nanomaterials for biomedical applications such as magnetic separation and drug delivery because of their non-toxicity, biocompatibility, and superparamagnetic nature. Recently, magnetic-plasmonic hybrid NPs such as Fe3O4@Ag and Fe3O4@Au have attracted much attention because of their separation and ultrasensitive detection [14,15,16].

Furthermore, SERS has recently drawn great interest as a powerful analytical tool for biomedicine, which allows highly sensitive biochemical analysis with multiplex and is much narrower than the fluorescence emission band [17,18,19,20]. Although SERS probes provide superior multiplexing analysis, they have relatively low temporal resolution owing to their slow imaging speed and relatively long acquisition time. Thus, the rapid recognition of many target biomarkers within a limited time is difficult to perform. To overcome this limitation, the combination of SERS and fluorescence is considered a promising technique, in which fluorescence is a quick indicator of the analytes, while SERS is used to distinguish specific targets in multiplex interactions. Recently, trifunctional NPs with SERS, magnetism, and fluorescence properties have been reported, which can provide a highly sensitive analytical tool in various biomedical applications [3, 21, 22]. Although these materials present excellent characteristics, their critical problems are fluorescence quenching, autofluorescence, and toxicity using organic dye and QD as fluorescence materials. Therefore, the development of biocompatible multifunctional nanocomposites is required for various biomedical applications.

In this study, we synthesized multifunctional nanocomposites of Ag-decorated Fe3O4 (Fe3O4–Ag) and Eu-doped Y2O3 (Y2O3:Eu3+) using high-energy ball milling (HEBM), and investigated their characteristics. The HEBM method is a one-pot synthesis, solvent-free or involves small amounts of solvents, environmentally friendly, and cost-effective. Furthermore, this method is conducted at room temperature, so does not require high-temperature treatment. The fluorescence-active Y2O3:Eu3+ NPs were conjugated with magnetic-SERS-active Fe3O4-Ag NPs to realize SERS-magnetic-fluorescence tri functions.

Experimental methods

Synthesis

Eu3+-doped Y2O3 nanoparticles (Y2O3:Eu3+ NPs)

Y2O3:Eu3+ NPs were synthesized using a planetary ball mill (Pulverisette 6 Fritsch, Germany) at room temperature, as previously described [23]. Yttrium oxide (Y2O3) and europium (III) nitrate hexahydrate (Eu (NO3)3∙6H2O) were used as starting materials, with 7 mol% Eu3+ added. The weight ratio of the sample to the ball was 50:1. The samples were milled for 120 min in an 80-mL zirconia jar at 500 rpm. To prevent overheating inside the mill pot, milling was conducted for 15 min and then rested for 15 min. The as-prepared powders were annealed at 800 °C for 1 h.

Synthesis of Ag-decorated Fe3O4 (Fe3O4-Ag) NPs

HEBM was used to synthesize Ag-decorated Fe3O4 NPs (Fe3O4-Ag NPs). Fe3O4 and AgNO3 were used as starting materials in the 1:1 mol% ratio. The complex power and zirconia (ZnO) ball had the weight ratio of 12:1. They were milled for 30 min in an 80-mL zirconia jar rotating at 400 rpm. The as-prepared powders were annealed at 400 °C for 1 h.

Synthesis of Fe3O4-Ag@Y2O3:Eu3+ nanocomposites

Fe3O4–Ag@Y2O3:Eu3+ mixtures were prepared by mixing the synthesized Fe3O4–Ag and Y2O3:Eu3+ at weight ratios of 1:1, 1:3, and 1:5. The mixtures were then milled using a planetary ball mill at room temperature. The Fe3O4–Ag@Y2O3:Eu3+ powders and zirconia balls had the weight ratio of 20:1. They were milled for 30 min in an 80-mL zirconia jar at 400 rpm.

Characterization

X-ray diffraction (XRD) of the samples was performed using a diffractometer (PANalytical, X'pert PRO MPD) with Cu Kα (λ = 1.54060 Å) radiation in the 2θ measurement range of 10°–80° at the scanning rate of 0.02°/s. The voltage and current of the acceleration were 40 kV and 30 mA, respectively. Field-emission scanning electron microscopy (FE-SEM, S-4800 Hitachi) equipped with energy-dispersive spectroscopy (EDS) at 15.0 kV was used to observe the morphology and elemental make-up of samples. A vibrating sample magnetometer (Lake Shore 7400, USA) was used to study the hysteresis loops and magnetic properties of the samples at room temperature with an applied magnetic field cycling between − 5000 and + 5000 Oe. Fourier transform infrared (FTIR) spectra were obtained in the 400–3800 cm−1 range using a Nicolet 6700 spectrophotometer (Sinco). Raman spectra were recorded using an XperRam F1.4 system (Nanobase Inc., Seoul, Korea) equipped with a 785 nm diode laser source. The laser power per unit area incident on the sample surface was 0.13 mW/cm2, and the exposure time was 5 s. All measurements were subjected to a baseline correction. The photoluminescence excitation (PLE) and emission (PL) spectra were measured using a FluoroMax-4 spectrofluorometer (Horiba Jobin Yvon Inc., Japan) at room temperature.

Results and discussion

Figure 1a–c display the XRD patterns of Fe3O4–Ag, Y2O3:Eu3+, and the Fe3O4–Ag@Y2O3:Eu3+ nanocomposite. The XRD result of the Fe3O4–Ag NPs contains the characteristic of Fe3O4 crystal planes 2θ = 30.1, 35.4, 43.0, 53.5, 57.1, and 62.7° corresponding to (220), (311), (400), (422), (511), and (440), and Ag cubic phase 2θ = 38.1°, 44.2°, 64.4°, and 77.4° corresponding to (111), (200), (220), and (311) (Fig. 1a). The circles and stars represent the Ag and Fe3O4, respectively. This is in good agreement with the standard XRD peaks of Fe3O4 (JCPDS 00-001-1111) and Ag (JCPDS 00-004-0783) phases, confirming the decoration of Fe3O4 with Ag NPs. Figure 1b presents the XRD pattern of the Y2O3:Eu3+ NPs. The 2θ values were 29.2°, 33.9°, 48.7°, and 57.8° corresponding to the (222), (400), (440), and (622) planes, respectively. This is in good agreement with JCPDS card no. 69-100-9014 of Y2O3 crystals. The absence of secondary phases confirmed the efficacy of the synthesis in transferring Eu3+ ions into the Y2O3 matrix over the entire range of Y3+ substitution levels. The XRD pattern of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites exhibit features of Fe3O4–Ag NPs and Y2O3:Eu3+ NPs, where the circles and stars indicate the phases of Fe3O4–Ag and Y2O3:Eu3+, respectively (Fig. 1c). These results imply that Fe3O4–Ag NPs and Y2O3:Eu3+ NPs were successfully conjugated.

Fig. 1
figure 1

XRD patterns of the a Fe3O4–Ag, b Y2O3:Eu3+, and c Fe3O4–Ag@Y2O3:Eu3+ nanocomposites

Figure 2a–c present the SEM images and EDS results of Fe3O4–Ag, Y2O3:Eu3+, and the Fe3O4–Ag@Y2O3:Eu3+ nanocomposite. The Fe3O4–Ag NPs show roughly spherical nanostructures with an average particle size of 30–50 nm. The presence of Fe, O, and Ag is confirmed through the EDS analysis, and the results are in good agreement with the initial element. Y2O3:Eu3 NPs present small, agglomerated grains. In EDS, the initial element O, Y was observed. The particle size was approximately 50 nm. For the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites, the particles present spherical shape and agglomerates of tiny particles. The average particle size was 50–100 nm. The EDS result confirms the presence of Fe, O, Ag, Y, and Eu, and is consistent with the XRD results.

Fig. 2
figure 2

SEM images and EDS results of the a Fe3O4–Ag, b Y2O3:Eu3+, and c Fe3O4–Ag@Y2O3:Eu3+ nanocomposites

Figure 3 displays the FTIR spectra of Fe3O4, Fe3O4–Ag, Y2O3, Y2O3:Eu3+, and the Fe3O4–Ag@Y2O3:Eu3+ nanocomposite. The absorption band observed at around 506–658 cm−1 for the Fe3O4 and Fe3O4-Ag NPs corresponds to Fe–O in the crystal lattice of Fe3O4 particles [24, 25]. The absorption band centered at 565 cm−1 for Y2O3 and Y2O3:Eu3+ can also be seen, which is assigned to Y–O stretching modes [26]. The absorption bands in the spectral ranges of 1200–1700 and 2855–2920 cm−1 are attributed to the C–O and C–H bond stretching vibrations, respectively [26, 27]. The broad absorption band centered around 3425 cm−1 is assigned to the stretching vibration of O–H [27]. For the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites, the FTIR spectrum presents the absorption peaks of Fe3O4–Ag and Y2O3:Eu3. This result also supports that Fe3O4–Ag and Y2O3:Eu3+ NPs are well combined.

Fig. 3
figure 3

FTIR spectra of the Fe3O4, Fe3O4–Ag, Y2O3, Y2O3:Eu3+, and Fe3O4–Ag@Y2O3:Eu3+ nanocomposites

Additionally, the magnetic properties of the samples were investigated. Figure 4a, b show the magnetic hysteresis loops of the Fe3O4, Fe3O4@Ag, and Fe3O4–Ag@Y2O3:Eu3+ nanocomposites with different Fe3O4@Ag and Y2O3:Eu3+ weight ratios of 1:1, 1:3, and 1:5, respectively. Compared with the Fe3O4 NPs, the saturation magnetization of the Fe3O4@Ag NPs decreased owing to the non-magnetic contribution of Ag. Furthermore, for Fe3O4–Ag@Y2O3:Eu3+ nanocomposites, the saturation magnetization was not only lower than that of the Fe3O4–Ag NPs, but clearly decreased with increasing concentration of Y2O3:Eu3+ NPs, owing to the diamagnetic contribution of the Y2O3:Eu3+ NPs. Although the saturation magnetization of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites is less than that of Fe3O4 and Fe3O4–Ag NPs, it is strong enough for effective magnetic separation. The inset of Fig. 4b shows a photograph of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites (weight ratio 1:5) dispersed in water with and without a magnetic field. When a magnet was placed close to the vial, the nanocomposites were attracted to the magnet very quickly and accumulated to the side of the vial near the magnet in ~ 20 s, and the solution became clear and transparent.

Fig. 4
figure 4

Magnetic hysteresis loops of the a a: Fe3O4, b: Fe3O4@Ag, c: Fe3O4–Ag@Y2O3:Eu3+ (R = 1:1), d: Fe3O4–Ag@Y2O3:Eu3+ (R = 1:3), e: Fe3O4–Ag@Y2O3:Eu3+ (R = 1:5), and b enlarged magnetic hysteresis loops of the ce. The inset of b presents a photograph of the Fe3O4–Ag@Y2O3:Eu3+ (R = 1:5) nanocomposites dispersed in water without and with a magnetic field

The photoluminescence efficiencies of Fe3O4–Ag@Y2O3:Eu3+ nanocomposites can be enhanced by increasing the Y2O3:Eu3+ concentration. Figure 5a, b present the PLE and PL spectra of Fe3O4–Ag@Y2O3:Eu3+ nanocomposites with different weight ratios of Fe3O4–Ag and Y2O3:Eu3+ powders, respectively. The PLE spectra of the samples were recorded in the spectral range of 150–350 nm at room temperature under the emission wavelength of 610 nm. All excitation spectra are dominated by a broad absorption band at 250 nm, which is attributed to the charge transfer that occurs from the ligand O2− ion to the central Eu3+ ions [28, 29]. The PL spectra of the samples were obtained in the spectral range of 500–700 nm at room temperature under the excitation wavelength of 250 nm. The PL spectra show a strong visible red emission at 610 nm and very weak peaks at 586, 591, and 629 nm at the excitation wavelength of 250 nm. The strong peak at 610 nm is attributed to 5D0 → 7F2, and the other weak peaks are assigned to the 5D0 → 7F0 (586 nm), 5D0 → 7F1 (591 nm), and 5D0 → 7F3 (629 nm) transitions of Eu3+ (see Fig. 6) [30, 31]. As expected, the PLE and PL spectra of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites increase with increasing Y2O3:Eu3+ concentration. Thus, it is important to determine the optimal dopant concentration for efficient multifunctional nanocomposite synthesis. The inset of Fig. 5b presents luminescence photographs of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites (weight ratio 1:5) under 365 nm ultraviolet lamp radiation; strong red fluorescence can be seen.

Fig. 5
figure 5

a Excitation and b emission spectra of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites at different Y2O3:Eu3+ concentrations [Fe3O4–Ag: Y2O3:Eu3+ (a.1:1, b.1:3, c.1:5)]

Fig. 6
figure 6

Energy level structure of the trivalent europium ion (with wavelengths for Y2O3:Eu3+)

The SERS activity of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposite substrate was examined using crystal violet (CV) as a Raman marker. We dropped 5 µL of 1 mM CV onto Al foil and 100 μM CV onto Fe3O4–Ag@Y2O3:Eu3+ (weight ratio 1:5) nanocomposites, dried them in air to assess the enhancing ability of the substrates, and then measured the Raman spectrum. Figure 7 presents the Raman spectra of CV deposited on the Al foil, as a reference, and that of the Fe3O4–Ag@Y2O3:Eu3+ substrate. The bands at 939 cm−1 were assigned to ring skeletal vibration [32]. The band at approximately 1172 cm−1 was assigned to in-plane C–H bending vibrations. The peaks at 1391 cm−1 correspond to N-phenyl stretching [33]; those at 1538, 1585, and 1620 cm−1 were assigned to ring C–C stretching [34]. The intensities of the Raman bands of the CV deposited on the Fe3O4–Ag@Y2O3:Eu3+ substrate show a clear improvement over the Al foil, as displayed in Fig. 7. This result implies that the Ag decorated on the Fe3O4 supports a strong surface plasmon. Therefore, Fe3O4–Ag@Y2O3:Eu3+ nanocomposites can be used as a highly sensitive analytical tool for various biomedical applications.

Fig. 7
figure 7

Raman spectra of crystal violet on the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites substrate and Al foil

Conclusions

We successfully synthesized multifunctional nanocomposites using HEBM. The developed Fe3O4–Ag@Y2O3:Eu3+ nanocomposites exhibit SERS, magnetic, and fluorescence properties. The saturation magnetization of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites was less than that of the Fe3O4–Ag NPs, although it was strong enough for effective magnetic separation. The photoluminescence spectrum of the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites revealed a strong visible red emission at 610 nm, attributed to the 5D0 → 7F2 electric dipole transition of Eu3+. Compared with the CV deposited onto Al foil, the intensity of the Raman bands of CV deposited on the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites showed a significant increase. Thus, the Fe3O4–Ag@Y2O3:Eu3+ nanocomposites can serve as a highly sensitive and selective probe for SERS-magnetic detection, and can be used as a visible fluorescence label in biomedical applications.

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Acknowledgements

This study was supported by the 2018 Research Fund of Chosun University.

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Back, H.E., Jung, G.B. Characterization of multifunctional nanocomposites assembled from Ag-decorated Fe3O4 and Eu-doped Y2O3. J. Korean Phys. Soc. 80, 1048–1053 (2022). https://doi.org/10.1007/s40042-022-00469-z

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Keywords

  • Multifunctional nanocomposites
  • Fe3O4–Ag@Y2O3:Eu3+ nanocomposites
  • High-energy ball-milling
  • Rare earth
  • Surface enhanced Raman scattering (SERS)