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. 2021 Oct 18;6(42):28334–28346. doi: 10.1021/acsomega.1c04526

Enhanced Visible-Light Absorption of Fe2O3 Covered by Activated Carbon for Multifunctional Purposes: Tuning the Structural, Electronic, Optical, and Magnetic Properties

Dahlang Tahir †,*, Sultan Ilyas †, Roni Rahmat †, Heryanto Heryanto †, Ahmad Nurul Fahri †, Mufti Hatur Rahmi ‡, Bualkar Abdullah †, Chol Chae Hong §, Hee Jae Kang ⊥
PMCID: PMC8552456  PMID: 34723030

Abstract

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Visible-light absorption is a critical factor for photocatalyst activity and absorption of electromagnetic (EM) interference application. The band gap of Fe2O3 is 2 eV, which can be increased by doping with a high-band-gap material such as carbon from activated carbon (AC) with a band gap of 4.5 eV for increased visible-light absorption. The porosity decreases from 88 to 81.6%, and the band gap increases from 2.14 to 2.64 eV by increasing the AC from 10 to 25%, respectively. The photocatalytic activity takes 120 min to produce a harmless product for 10–20% AC, but 25% AC shows 89.5% degradation in only 90 min and the potential to attenuate the EM wave up to 99% due to the RL being below −20 dB. The second- and third-cycle degradation achieved by the composite Fe2O3–AC having 25% AC is 88.2 and 86.5% in 90 min, respectively. The pore of the surface state of AC contains a trapped charge, and interaction occurs between the charge (electron/hole) and O2 or H2O to produce OH and superoxide (O2–) radicals. These radicals move inside the molecule of the pollutant (methylene blue (MB)) to break up the bond, with the final products being H2O and CO2. The X-ray photoelectron (XPS) spectra show that oxygen plays a key role in the interatomic bonding with Fe, C, and MB atoms. The best absorption of EM interference is −21.43 dB, with degradation reaching 89.51% in only 90 min for 25% AC due to its higher band gap and anisotropy constant. Fe2O3–carbon is a multifunctional material for the green environment because of its electromagnetic interference absorption and photodegradation of wastewater.

1. Introduction

The lifestyle of humans in the modern and digital era has increased the demand for textile and electronic products, leading to the development of new industries for supporting the demand.1−4 The textile industry has been contributing to environmental pollution due to the increasing use of toxic chemicals in the processing stage,5−9 which is of concern, especially the wastewater treatment before disposal.10 About 40% of the dyes used globally contain organic synthetic bound chlorine, which affects the environment by reducing oxygen concentration and preventing light at the water surface, consequently damaging the aquatic ecosystem.11,12 This in turn cause diseases in humans, who are exposed to the organic synthetic bound chlorine through the water and contaminated food. The chlorine’s effects can vary from cough and chest pain to water retention in the lungs,13,14 and irritation in the skin,15 eyes,16 and the respiratory system.17−19 The increasing demand for electronic devices has consequently increased their production, which has directly led to increase in electromagnetic interference (EMI) waves.20−26 EMI has been identified as a new type of pollution that interferes with electronic communications devices and causes threats to human health.20−24,27−29 Humans can absorb the pollution and radiation from the electromagnetic (EM) waves; therefore, scientists globally are looking for a way to efficiently shield and absorb these EM waves. There are two main problems with increase in the population globally, which have side effects on human health, they are the availability of clean water and energy. Therefore, innovations with regard to manufacturing efficient energy, water, and chemicals by using multifunctional materials for wastewater treatment and absorption of EM waves are crucial. This innovation can support sustainable development goals (SDGs): point 6 and point 7.3

The innovations in multifunctional materials have led to photodegradation of wastewater and EM wave absorption by tuning the electronic (band gap), magnetic, and optical properties to increase the absorption from UV light to visible light.20−26,30−32 A semiconductor material has unique properties that make it easy to tune these properties, so it is suitable for electromagnetic wave absorption and photocatalyst applications.33−36 Among the semiconductor materials, one of the binary semiconductors is Fe2O3, with a band gap of about 2 eV, natural abundance, electrochemical stability, and low toxicity.37,38 The limitations of this material are its poor electrical conductivity and optical properties for absorbing the solar spectrum only for wavelengths >600 nm. By doping with high-band-gap materials, the optical absorption is enhanced in the visible regions.39 Activated carbon (AC) increases the band gaps of CuO23 and Fe3O420 for absorbing EM wave interference.21,24,40 AC is used to tune the structural, magnetic, and optical properties of the semiconductor by doping it with various materials22,25,26,41 depending on the application.23,42−46 In our previous study, we successfully used Co/Fe2O3–AC for EM absorbers,47 but the physical phenomena between Fe2O3 and AC are still not fully understood. Several questions exist regarding the relations between the optical, magnetic, electronic, and structural properties that support the applications of multifunctional materials. What relation between these properties supports the capability of Fe2O3–AC in absorption of EM and photodegradation of wastewater? What is the effect of carbon on the performance of Fe2O3–AC in multifunctional purposes? The following approach (explained in the Materials and Experiment section) addresses these questions regarding the Fe2O3–AC materials.

In this study, the optical band gap of Fe2O3 is increased by doping with the carbon from AC for enhancing visible-light absorption in the photodegradation activity and absorption of EM waves. The relations between the structural, electronic, magnetic, and optical properties in supporting the multifunctional applications of the semiconductor Fe2O3–carbon are analyzed and discussed. Various amounts of carbon affect differently the structural and chemical bonding properties of Fe2O3,26,48−51 which were identified using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). The optical properties (refractive index (n and k)) and dielectric function (ε) of the semiconductor Fe2O3–carbon were determined from the quantitative analysis of the FTIR spectra using Kramers–Kronig (KK) relation. This method was successfully applied for the following materials: the composite cement/BaSO4/Fe3O4,52 composite geopolymer fly ash–metal,53 Co/Fe2O3–AC,47 nanoparticle Zn(OH)2,54 composite Fe/CNs/PVA,55 bioplastics (SPF/starch/chitosan/polypropylene),56 and composite nanocrystalline carbon–lignin/zinc oxide.57 The magnetic properties are measured using a vibrating sample magnetometer (VSM) for various amount of carbon in Fe2O3. X-ray photoelectron spectroscopy (XPS) was used for identifying the interactions and bonding states at the interatomic level. Reflection electron energy loss spectroscopy (REELS) was used for determining the optical band gap.20,25,26,39,41,49−51,58 The EM wave absorption performance was analyzed using the vector network analysis (VNA) in the frequency range from 2.5 to 8 GHz. For photocatalytic performance, the UV–vis spectra were recorded every 30 min using the irradiation from a halogen lamp with methylene blue as a model of wastewater.

The proposed processes for increasing the efficiency of the composite materials in this study are the following:

  • 1.

    To enhance visible-light absorption, the band gap is increased by increasing the amount of AC determined from the low-loss energy region of the REELS spectra (the basic idea can clearly be seen in Figure 1).

  • 2.

    The stable bonding is due to AC’s hexagonal structure, which quickly spreads and converts the EM to thermal energy when entering the composite (the basic idea can clearly be seen in Figure 1).

  • 3.

    Recombination between the charges (electrons and holes) is reduced during the photodegradation process in the magnetic pore (of AC) by trapping the charge and generating the oxidants hydroxyl radical (OH) and superoxide anion radical (O2–). This process, via photoelectrochemical decomposition of H2O and O2, consequently increases the photodegradation performance in the visible-light region (the basic idea can clearly be seen in Figure 2).

Figure 1.

Figure 1

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Illustration of the mechanism for enhancing visible-light absorption by varying the amount of activated carbon (AC). When the EM wave enters the material, the interaction occurs with the atoms, and the energy spreading into the small waves produces vibration of the atoms and the lattice structure, and some of the energy is converted to thermal energy.

Figure 2.

Figure 2

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Proposed photodegradation process. The photon energy absorbed by the electron in the valence band moves to the conduction band; the remaining hole, which goes to the surface of the material, is captured by the magnetic pore for generating OH and the superoxide anion radical (O2–) via photoelectrochemical decomposition of the H2O and O2 molecules for breaking the chemical structure of the pollutant, finally giving a harmless product.

2. Results and Discussion

Figure 3 shows the XRD full spectrum (a), the enlarged diffraction peaks (104) and (110) (b), and the FTIR spectra (c) for Fe2O3–carbon. The intensity of the diffraction peak for the composite Fe2O3–carbon shows that the Fe2O3 diffraction peak is dominant as expected, due to the composite’s high concentration. For further analysis, the Scherrer and size strain plot (SSP) methods were used in the XRD pattern to determine AC’s effect on the structural properties of the composites. The FTIR pattern shows the dominant peaks at a low wavenumber, usually for the vibration mode of metals.20 From 400 to 550 cm–1 is the vibration between Fe2O3 and other O or C atoms. The peaks arise from C bonding with −CH, −OH, and =C, and the O–H vibration mode from another small transmittance. The FTIR pattern is used to further determine the optical properties and dielectric function of the composite semiconductor Fe2O3–carbon for the strong peaks at the wavenumbers (ω) from 400 to 550 cm–1.59 For these purposes, Kramers–Kronig (KK) relation is used in the quantitative analysis of the FTIR pattern.

Figure 3.

Figure 3

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(a) X-ray diffraction (XRD) full spectrum, (b) enlarged diffraction peaks (104) and (110), and (c) Fourier transform infrared (FTIR) spectra for the composite Fe2O3–carbon as a function of the amount of carbon. We have included ICDS 98-008-8414 for comparison.

The XRD diffraction pattern was used to determine the physical quantity, the full width at half-maximum (βhkl), the wavelength source of the radiation (λ), which in this study was 1.54056 Å for Cu Kα, and the angle (θ) of the diffraction peaks. βhkl was determined from the instrumental broadening (βinstrumental) by using Gaussian correction compared with the data for the standard crystalline Si.30,32,60−63 The relation between βhkl, βinstrumental, and βmeasures is represented by30

2. 1

βhkl was used as an input parameter to determine the crystallite size using the Scherrer equation as follows

2. 2

The dislocation density calculated from the crystallite size D is presented in Table 1, and is related to the defects in Fe2O3–carbon crystal structure, lattice parameter, volume crystal, porosity, and bond length.

2. 3
2. 4
2. 5

where V is the volume, u is an internal parameter, and L is the bond length. The porosity is >80% for all composites, indicating the potential for absorbing the electromagnetic waves.23

Table 1. Quantitative Analysis of the XRD Spectra for Determining the Crystallite Size, Lattice Parameter, and Porosity of the Composite Semiconductor Fe2O3–Carbon.

      lattice parameter (Å)
        
sample ID D (nm) a c volume (VCal) ratio (c/a) dislocation density (1/D2) (nm–2) porosity (%) bond length (Å)
Fe2O3 15.33 5.02 13.71 299.4 2.73 0.0043 89.87 4.04
10% AC 11.06 5.00 13.63 295.1 2.73 0.0082 88.02 4.02
15% AC 14.01 5.04 13.70 301.4 2.72 0.0051 85.46 4.04
20% AC 12.29 5.00 13.64 295.5 2.73 0.0066 82.72 4.02
25% AC 15.76 4.97 13.58 290.5 2.73 0.0040 81.63 4.00
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Figure 3b shows that the peaks were shifted to a higher 2θ; the porosity decrease is attributed to the carbon content increase in the composite, which may be due to the oxygen content decrease and the C atoms replacing some of the O atom positions in bonding with Fe. Therefore, the solid solution composite probably formed CxFeO1–x. The porosity linearly affects the surface area, which affects the properties of the material. This implies that the amount of C in the composite semiconductor Fe2O3–carbon and the formation of vacancies in the solid solution are increasing. The oxygen might decrease more probably around the Fe atoms rather than the C atoms. This is due to the differences in valence electrons between the C and Fe atoms. The oxygen decrease due to the bonds among them causes weak asymmetry of the local bond. The local bonding between a C atom and another C atom is dominantly covalent and metallic, and has an ionic character in a few clusters of crystal structures.64 For 15% AC, the shift to the lower 2θ, probably due to the crystal structure’s local strain and bond asymmetry from the C atoms, was not in the stable position in the lattice structure.20,24,30

The C atoms neighboring the Fe atoms would experience weak covalent bonds compared with the neighboring O atoms. This result implies that C bonding with O atoms plays an essential role in determining the lattice parameters. In particular, the carbon content significantly affects the lattice parameter.20−22,30,32,58

The microstrain (ε) contributes to the broadening βstrain = 4ε tan θ66−68 and the full width at half-maximum (β) as follows

2. 6

where D is the crystallite size (nm), ε is the microstrain, β is the full width at half-maximum, and k is 0.94.

The models for the quantitative analysis of the XRD pattern for determining the structural properties are used at a high diffraction angle for high-accuracy results, and the size strain plot (SSP) method is applied at a low diffraction angle for better accuracy.61,65,68 The SSP model is described in detail as30,32,63,65,69,70

2. 7

where d is the spacing between the atoms (Å) and ε is the microstrain. The contribution of the isotropic lattice is determined from the Gaussian functions and D is determined from the Lorentz functions. Figure 3a shows the Scherrer method and Figure 3b shows the SSP plot for the Fe2O3/AC composite; the corresponding structural properties are shown in Table 2. Figure 4 shows clearly the difference between the Scherrer and SSP methods; all data (indicated by the dotted lines) in the SSP plot shown close to the solid line indicate the high accuracy of the calculation methods.

Table 2. Quantitative Analysis of the XRD Spectra by Applying Scherrer and Size Strain Plot (SSP) Methods for Determining the Structural Properties of the Composite Semiconductor Fe2O3–Carbon.

  Scherrer method SSP
sample ID D (nm) D (nm) E (10–3) σ (Mpa) u (Kj m–3)
Fe2O3 15.33 31.51 0.17 38.25 3.18
10% AC 11.06 25.02 0.11 24.89 1.40
15% AC 14.01 27.01 0.30 66.47 10.13
20% AC 12.29 23.99 0.29 63.09 9.30
25% AC 15.76 25.27 0.47 99.76 23.69
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Figure 4.

Figure 4

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(a) Scherrer and (b) size strain plot (SSP) methods for the analysis of the XRD spectra in Figure 3a. Optical properties: (c) refractive index (n) and extinction coefficient (k), and (d) the real (ε1) and imaginary parts (ε2) of the dielectric function from quantitative analysis of the FTIR spectra in Figure 3c.

The D average and ε determined from the Scherrer and SSP methods are shown in Table 2. Figure 4a,b, and Table 2 show that the D from the Scherrer method is smaller than that from the SSP method due to the effect of ε and the distance between the atoms included in the SSP method.30,32,63

The FTIR spectra were used for determining the refractive index (n), extinction coefficient (k), and dielectric function based on the following equations. First, the pattern was converted from transmittance T(ω) to reflectance R(ω)71−82

2. 8
2. 9

The reflectance pattern R(ω) is the input spectra used for determining n(ω) and k(ω) as follows73,74

2. 10
2. 11

where the phase change φ(ω) is the reflection of the photon after traveling inside the sample

2. 12

The φ(ω) is made more simple for computation by applying the KK relation73,75

2. 13

where j is the series of the wavenumber; if j is an odd number, then the i values are 2, 4, 6, 8, ..., j – 1, j + 1 and if the wavenumber j is even, the i values are 1, 3, 5, 7, ...,  j – 1, j + 1, ...; Δω = ωi+1 – ωi. The n(ω) and k(ω) values from the analysis of FTIR spectra are shown in Figure 4c. The lower intersection wavelength point between n(ω) and k(ω) is the transverse optical (TO) mode and the higher one is the longitudinal optical (LO) phonon vibration mode, as clearly shown in Figure 4c.

The dielectric functions for the real part ε1(ω) and imaginary part ε2(ω) were determined as follows

2. 14
2. 15

Figure 4d shows the dielectric function in the form of real (ε1(ω)) and imaginary parts (ε2(ω)). At the surface layer, the breaking of the interatomic bonding happens, and the new structure formed is indicated by the dielectric function peaks in the range from 430 to 450 cm–1.76 Δ(LO-TO) is the distance between two optical phonon modes, which decreases on increasing the concentration of carbon in the composites as presented in Table 3, probably due to the nonuniformity of the lattice in the composite semiconductor Fe2O3–carbon, and consequently the less stable structure.77,78

Table 3. Band Gap Derived from the REELS Spectra in Figure 5aa.

sample band gap (eV) To (cm–1) Lo (cm–1) Δ(Lo-To) (cm–1) ε1 (cm–1) kr R2
Fe2O3 2.00 446.42 491.09 44.67 432.85 0.020 0.998
10% AC 2.14 444.49 491.94 47.45 431.04 0.023 0.992
15% AC 2.30 449.30 491.52 42.22 436.80 0.022 0.955
20% AC 2.50 448.34 490.26 41.92 434.65 0.027 0.977
25% AC 2.64 448.64 490.68 42.04 435.08 0.030 0.987
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a

Transverse optical phonon (To) and longitudinal optical phonon (Lo), and the real (ε1) and imaginary parts (ε2) of the dielectric function from the quantitative analysis of the FT-IR spectra in Figure 3c. The rate constant (kr) and correlation coefficient values (R2) for Fe2O3 and the composite semiconductor Fe2O3–carbon for 10, 15, 20, and 25% AC from the degradation analysis in Figure 6c,d.

The details of determining the band gap from the low-loss region of the REELS spectra have been reported in some previous studies.20,25,26,39,49,50,79,80Figure 5a shows the band gap of Fe2O3–carbon determined from the low-loss region’s REELS spectra. The corresponding values of these band gaps are shown in Table 3. The band gap increases from 2.0 eV for Fe2O3 to 2.64 for 25% AC due to the amount of AC, as the more vital interaction between the C 1s from AC with the Fe 3d and O 2p from Fe2O3 makes the top of the valence bands become thin.48 The bottom of the conduction bands is also changed after the introduction of AC into the composite Fe2O3–carbon. The mixing of the C 1s states at the valence band edge decreases the valence bandwidth; the increase of the band gap increases the amount of AC probably due to the formation of C1–x(Fe2O3)x. These results increase the photon excitation energy, which contributes to the generation of electrons and holes, consequently increasing the absorption and degradation ability.81 The generated electrons and holes move to the surface of the semiconductor Fe2O3 and jump to the pore as a charge trap for decreasing the recombination.82

Figure 5.

Figure 5

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(a) Band gap determined from the low energy loss region of the reflection electron energy loss spectroscopy (REELS) spectra at primary energy Eo = 1500 eV. (b) Magnetic properties determined by VSM, and (c) reflection loss properties of Fe2O3–carbon for various amounts of carbon (10%, 15%, 20%, and 25% AC).

Figure 5b shows the magnetic properties measured at room temperature using a vibrating sample magnetometer with applied field −10 kOe < H < 10 kOe. From the hysteresis loops, the coercivity (Hc), saturated magnetization (Ms), and remanent magnetization (Mr) were analyzed and used to determine the remanent ratio (R) and isotropic constant (K1); the corresponding results are shown in Table 4. The composite Fe2O3–carbon in this study shows a multidomain soft ferrimagnetic nature due to the high coercivity (Hc) ranging from 1323.75 Oe for 10% AC decrease to 444.40 Oe for 25% AC, and a low saturation magnetization (Ms) ranging from 0.390 emu/g for 10% AC increase to 0.524 emu/g for 25% AC. The short-range exchange interaction leads to a more substantial magnetic ordering of all spins from the AC, resulting in increase in the Ms.83

Table 4. Magnetic Properties and Reflection Loss Properties Determined from Figure 5b,c, Respectively, for the Composite Semiconductor Fe2O3–Carbon.

sample HC (±0.05 Oe) MR (±0.05 emu/g) MS (±0.05 emu/g) K1 MR/Ms thickness (mm) RL (dB) frequency (GHz) bandwidth (GHz)
10% AC 1323.75 0.157 0.390 285.13 0.40 2 –17.04 6.16 2.67
3 –18.38 6.18 2.71
15% AC 945.54 0.151 0.425 200.93 0.36 2 –17.98 6.18 2.92
3 –18.39 5.57 3.01
20% AC 453.86 0.150 0.514 116.64 0.29 2 –17.17 5.14 3.27
3 –19.42 5.12 3.28
25% AC 444.40 0.149 0.524 116.43 0.28 2 –19.96 5.53 3.02
3 –21.43 5.54 2.84
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The ratio (R) between Mr and Ms decreases from 0.40 to 0.28 on increasing the amount of AC from 10 to 25%, respectively, consistent with the Mr decreasing from 0.157 emu/g to 0.149 emu/g due to the decrease of the multidomain soft ferrimagnetic materials. The value of R < 1 indicated the multidomain structure of all composites in this study and decreased with increase in the amount of AC due to the foreign carbonaceous phase that randomly influenced the magnetic dipole interaction orientation.84 The anisotropy constant (K1) was calculated by the Brown relation K1 = (Hc + Ms)/2, and the value decreased with the increase of the amount of AC, indicating the distribution of AC atoms in the Fe octahedral site of the lattice structure.83 The Fe–O bond becomes weaker with increase in the amount of AC atoms up to 25% by decreasing the lattice parameters.85,86

With AC increase, the Hc value was decreased, which is attributed to the carbon atoms creating a minor destruction in the lattice of the hexagonal structure of the ferrites.87 On substituting another small atom, the ionic radius increase in the carbon in the composite semiconductor Fe2O3–carbon may create more destruction within the lattice, resulting in a decreased magnetic crystalline anisotropy constant (K1). Hence, the decrease in coercivity and saturation magnetization values for increasing substitution of carbon atoms may be due to the carbon atoms preferring to fill the Fe ions’ octahedral site compared with the O ions. These phenomena have been identified as decreasing the MR and R due to the exchange interactions and the interatomic local strain increase at the octahedral sites.85−87

The composite shows reflection loss properties in Figure 5c, and the quantitative data shows in Table 4 that the thickness of the composite is 2 mm and 3 mm. For reflection loss (RL) of the composite below −10 dB, an EM absorption of 90% and RL below −20 dB absorbing 99% of the EM wave indicated excellent absorption properties.87 The increased RL caused an increasing amount of carbon (AC) due to the local strain. The exchange interactions increase at the octahedral sites as the MR and R-value decrease in the composite Fe2O3–carbon. In Figure 5c, the RL for thickness 3 mm increase from −18.38 to −21.43 dB for increasing from 10 to 25% AC, respectively, and the bandwidth increases from 2.71 GHz for 10% AC to 3.28 GHz for 20% AC and decreases to 2.84 GHz for 25% AC. It indicates that the efficiency for absorption of EM wave pollution and radiation increases from 90% for RL < −10 dB to 99% for RL < −20 dB. The thickness of 2 mm with the addition of AC increases the bandwidth, and the RL fluctuates slightly but is not much different from 3 mm. The composite Fe2O3–carbon reflected the electromagnetic waves, indicating the shielding of EM pollution and radiation by the frequency above or below the operating frequency bandwidth.

Figure 6 shows the XPS core level of Fe2O3 and composites Fe2O3–AC for Fe 2p (a), O 1s (b), and C 1s (c), which indicates the presence of carbon and Fe2O3 in the composites. Figure 6a shows two prominent peaks at ∼711 and ∼724 eV that denote the Fe 2p3/2 and Fe 2p1/2 electron binding energy, respectively, and the satellite that exists between these two prominent peaks is the fingerprint of the electronic structure of Fe3+, which is in agreement with the literature and shows the existence of Fe2O3.20,88 O 1s core-level spectra show the peak formation of C–O and C–OH bonding located at 529.62 and 531.44 eV, respectively. Figure 6a,b shows no noticeable change with the addition of AC up to 25% for the composites, which indicates that the Fe2O3 has a strong effect on the composite. The C 1s of Fe2O3 shows two peaks at 284.39 and 285.39 eV that contribute to the formation of Fe–C and C–C bonding, respectively. It is clearly shown in Figure 6c that the addition of AC up to 25% influences the formation of each bonding. The addition of AC then creates a new peak at ∼287 eV, which indicates the formation of Fe–O–C bonding but does not increase further following the addition of AC in the composite. The peak intensity of C–C bonding increases following the addition of AC in the composite, while the Fe–C bonding decreases. It is concluded that oxygen has a primary role in binding with the Fe and the C in the composite. The formation of the composite Fe2O3–AC has been confirmed from the XPS and REELS spectra.

Figure 6.

Figure 6

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X-ray photoelectron spectroscopy (XPS) core-level spectra for Fe2O3–carbon with various amounts of carbon (10, 15, 20, and 25% AC). (a) Fe 2p, (b) O 1s, and (c) C 1s.

The photocatalytic properties of the samples are shown in Figure 7a–d. The first-order degradation rate constant k is determined using Inline graphic, where C0 is the absorbance before the radiation and Ct is the absorbance after the applied radiation for time t.48Figure 7a shows the pollutant (methylene blue) before and after irradiation every 30 min. The pollutant’s absorbance becomes harmless as long as the irradiation is applied, which is more apparent than the pollutant’s maximum absorption point. The percentage of degradation is shown in Figure 7b, and the degradation rate constant is shown in Figure 7c,d. The degradation of the pollutant by the semiconductor Fe2O3–carbon increases with addition of AC in the composites. As shown in Figure 7b, for 25% AC, the degradation reaches 89.51% only in 90 min, whereas other samples need around 120 min to yield the harmless product. Figure 7c,d shows a plot of the Inline graphic versus time degradation for all samples, where the slope is used for determining k and correlation coefficient (R2) values, as shown in Table 3. The best performance for the degradation indicated by the highest rate constant is for the semiconductor Fe2O3–carbon with 25% AC. This is due to the higher band gap with an additional carbon in the semiconductor Fe2O3–carbon, suppressing the recombination of the electron–hole pair when irradiated.48,89 A combination of C 1s from AC with Fe 3d and O 2p will facilitate the generation of photo-induced electrons and suppress the recombination of the charge (electron–hole) pairs; consequently, the photocatalytic activity will increase.26,90,91 The increase of the carbon atom in the carbon-based magnetic materials will significantly increase the photocatalytic activity due to the destruction of the lattice, which is indicated by the decrease in the magnetic crystalline anisotropy constant (K1) and the coercivity.92−94 The C 1s states at the valence band edge increase with increasing carbon content based on the formula C1–x(Fe2O3)x, which may suppress the recombination of electron–hole pairs.

Figure 7.

Figure 7

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(a) Absorbance from UV–vis spectra and (b) degradation ability determined from the equation Inline graphic. The kinetic curve of the photocatalytic degradations (c) by Inline graphic and (d) Inline graphic for Fe2O3–carbon for various amounts of carbon (10, 15, 20, and 25% AC).

Less electron–hole recombination led to formation of more radical molecules and broke the pollutant bonding, thus yielding a harmless product.95 The electronic, magnetic, structural, optical, and photocatalytic properties of Fe2O3 can be tuned by adjusting the amount of carbon added, leading us to a promising multifunctional material for electromagnetic wave absorption/shielding and textile industry wastewater degradation. The novelty and photodegradation efficiency of this study compared with other references96−105 can clearly be seen in Table 5. The effect of AC concentration shows the highest efficiency as 93.76% for 20% AC but takes 120 min, compared with that of 25% AC, which is 89.51% but takes only 90 min.

Table 5. Comparison of the Synthesis Methods of the Materials and the Degradation Performance (%) of the Previously Reported Materials Containing Fe2O3 Doped with Various Materials-Based Photocatalysts with the Fe2O3–AC in this Study by the Simple Mechanical Alloying Method.

type of photocatalyst synthesis method photocatalytic application degradation performance reference
FeS2/Fe2O3 heat treatment carbamazepine 65% (by adding Cr (IV)) Guo et al.96
α-Fe2O3/rGO heat treatment and ultrasound method congo red 60% Wang et al.97
Fe2O3/rGO hummers method and Heat treatment 4-nitrophenol 98% Sathish Mohan et al.98
BiVO4/ α-Fe2O3 in situ growth method tetracycline ∼75.8% Ma et al.99
Fe3N/Fe2O3/C3N4 facile single-step preparation method rhodamine B 98% Padervand et al.100
KNbO3/α-Fe2O3 hydrothermal/solvothermal route methylene blue 89% Farooq et al.101
Fe2O3/GO/WO3 green method and ex situ method phenol 95.4% Mohamed et al.102
ZrO2/Fe2O3/RGO hydrothermal route and Hummers method congo red 98.43% Anjaneyulu et al.103
ZnO/Fe2O3 sol-gel method metronidazole 99% Davari et al.104
CuO/α-Fe2O3/γ-Al2O3 facile wet chemical route methylene orange 98% Kanwal et al.105
Fe2O3/25%AC simple mechanical alloying methylene blue 89.51 present study
Fe2O3/20%AC simple mechanical alloying methylene blue 93.76 present study
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Figure 8 shows the relation of the structural (D), magnetic (Hc), and optical properties (Δ and band gap) with the degradation performance (Deg.) and reflection loss (RL) for attenuating the EM waves. The magnetic property and the Δ decrease with increase in the amount of carbon, but the ability to attenuate the EM waves (RL) in contrast to the band gap indicates that the carbon successfully acts as a net by covering Fe2O3. The photocatalytic activity takes 120 min to produce a harmless product for 10 to 20% AC, but 25% AC shows 89.5% degradation in just 90 min and shows the potential to attenuate the EM waves up to 99% due to the RL being below −20 dB. The second- and third-cycle degradation of the composite Fe2O3–AC for 25% AC are 88.2 and 86.5% in 90 min, respectively. This study shows the high potential of the composite Fe2O3–AC for multifunctional purposes, photocatalytic activity, and as a very good EM absorber for wave applications.

Figure 8.

Figure 8

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Relation between the structural (D), magnetic (Hc), and optical properties (Δ and band gap) and the ability to attenuate the electromagnetic wave (RL) and the degradation performance (Deg.).

3. Conclusions

The semiconductor Fe2O3–carbon was used to successfully tune the structural, optical, band gap, and magnetic properties in the analyses by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), reflection electron energy loss spectroscopy (REELS), X-ray photoelectron spectroscopy (XPS), and a vibrating sample magnetometer (VSM), respectively. The EM wave absorption and removal of dye waste performance were analyzed using vector network analysis (VNA) and ultraviolet–visible (UV–vis) spectroscopy, respectively. The band gap linearly increased up to 2.64 eV by increasing the carbon content up to 25%, due to the interaction of C 1s with Fe 3d and O 2p affecting the top of the valence bands and making the band gap narrower in the form of C1–x(Fe2O3)x. These results increase the photon excitation energy, which contributes to the generation of electrons and holes, consequently increasing the absorption and degradation ability. The coercivity decreases on increasing the amount of AC due to the small atomic radii of the carbon inserted into the ferrite’s hexagonal structure. It creates a small wreck in the lattice, decreasing the K1 and Hc. The decrease in saturation magnetization occurs due to the nonmagnetic atoms of AC preferring to occupy the octahedral site of Fe ions rather than the O ions, leading to decreased MR and R, and increasing the local strain and exchange interactions at the octahedral sites. The best reflection loss is −21.43 dB at 5.54 GHz, and a degradation of up to 89.51% is achieved in only 90 min by 25% AC due to the higher band gap, which contributes to suppressing the recombination of the electrons and holes. These results indicate that the composite semiconductor Fe2O3–carbon from AC is a promising material for absorption of electromagnetic wave radiation and photodegradation of wastewater by tuning the structural, optical, and magnetic properties.

4. Experimental Section

Iron (III) oxide (Fe2O3) with a particle size of 50–100 nm and trace metals basis of 97% was purchased from Sigma Aldrich. Activated carbon (AC) with an average diameter of <10 μm, purity of >95%, and surface area of >240 m/g was purchased from PT. Cahaya Indo Abadi, Indonesia, and poly(vinyl alcohol) (PVA) with purity 99.5% was purchased from Merck.

The experimental procedure and the characterization system of XRD and FT-IR spectra were similar to those in the previous study.21,23,48,106 The magnetic studies were performed with a vibrating sample magnetometer (VSM) 1.2 H type from Oxford Instruments.20,23 The EM absorption was measured using a VNA (Vector Network Analyzer) (Rohde & Schwarz ZVHB) with the frequency range from 2.5 to 8 GHz, and the absorbance for every 30 min of irradiation was measured from the UV–vis (ultraviolet–visible) spectra (Shimadzu UV–vis Spectrophotometer UV-1800).20,21,23,30 The characterization by REELS was similar to that in our previous paper.20,23

For photocatalytic activity, the radiation source was a halogen lamp (300 W, OSRAM 645, Germany) and the measurement was done every 30 min. The pellet samples were suspended in 50 mL of methylene blue with a concentration of 1 × 10–5 M, and the distance from the halogen lamps was about 30 cm. The absorption spectra were recorded using an ultraviolet–visible (UV–vis) spectrophotometer, Shimadzu UV-1800.48

Acknowledgments

This work was supported by the PT (Penelitian Terapan) 2021 grant 752/UN4.22/PT.01.03/2021 funded by the DIKTI/BRIN, Indonesia.

The authors declare no competing financial interest.

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