Developed and characterization of a novel Cd doped CeO2 nanofilm and application of pesticide removed by photodegradation

doi:10.21203/rs.3.rs-3615189/v1

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Developed and characterization of a novel Cd doped CeO₂ nanofilm and application of pesticide removed by photodegradation

https://doi.org/10.21203/rs.3.rs-3615189/v1

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Cadmium (Cd) doped cerium oxide (CeO₂) films were prepared by ultrasonic spray pyrolysis (USP) technique. The structural, surface and optical properties of the prepared Cd doped CeO₂ films were investigated. All of the films were polycrystalline in exhibiting a cubic fluorite structure. In addition, the optical band gap obtained using the UV data ranged from 3.23 to 3.52 eV. For Cd doped CeO₂ films, Raman scattering, in which the multi-peak setting of the first optical longitudinal mode was observed, indicates the Raman shift of the characteristic peak in the ~ 461 cm^− 1 range. In addition, the photodegradation capacities of Cd doped CeO₂ films were investigated in pesticides removed polluting human and environmental health. As a result, the proposed Cd doped CeO₂ thin films show very high photocatalytic activity for the removal of important pollutant as Methyl Orange dyestuff. Consequently, Cd doped CeO₂ film could be easily reused for five cycles without significant change in the photocatalytic activity.

CeO2 film

Photocatalytic

X-ray diffraction

Raman spectroscopy

optical properties

ultrasonic chemical spray pyrolysis technique

Methyl Orange

Today, environmental pollution has become an element that threatens human health worldwide, along with the increase in urbanization and industrialization. Wastes from industrial plants are the biggest source of environmental pollution. These pollutants must be removed or even destroyed for human and environmental health. For this, different methods are used, especially for the removal of substances like dyestuffs. In recent years, the studies of the purification of organic pollutants by photocatalytic degradation from water by using semiconductor materials have attracted attention [1–3]. Semiconductor photocatalysts are one of the promising technologies as an alternative to classical methods for solving problems such as air and environmental pollution. Technologically, there has been an increased interest in techniques to improve the properties of films used in devices. Cerium oxide (CeO₂) is non-toxic, so it is bio-compatible, and safe. CeO₂ finds many applications in catalysts and catalyst supports [1, 2], cosmetics materials [3], ceramic materials [4], oxygen gas sensors [5], solid oxide fuel cells [6] and fluorescent materials [7]. CeO₂ show catalytic activity in many chemical reactions, due to the property high oxygen storage capacity. CeO₂ is of great interest due to its physical and chemical properties [8]. CeO₂ thin films have been obtained by many methods such as sol–gel process [9], sonochemical synthesis [10], gas condensation [11] and hydrothermal synthesis [12], spray pyrolysis [13–17], electron beam evaporation [18, 19], sputtering [20], pulsed laser deposition [21, 22], chemical vapor deposition [23, 24]. In this study, the cadmium (Cd) doped CeO₂ films have been constructed using ultrasonic spray pyrolysis (USP) technique. This technique is a simple technique for obtaining low cost thin films [25, 26]. Then, Cd doped CeO₂ thin films has been examined in detail using X-ray powder diffraction (XRD), scanning electron microscope (SEM), atomic force microscope (AFM), ultraviolet–visible spectroscopy (UV-Vis), photoluminescence (PL) and raman spectroscopy techniques. Finally, photocatalysis capacity under UV/visible/sunlight was investigated in Methyl Orange dyestuff removal to increase the migration of carriers during excitation of Cd doped CeO₂ compound, which is chosen as a photocatalyst with light effect during excitation. As a result, Cd doped CeO₂ thin films can remove dyestuff, which are an important class of pollutants, in a simple, fast, low-cost, and high removal rate.

USP technique is established on the theories and configurations presented in the literature [25, 26]. The experimental setup used is shown in Fig. 1. First of all, cerium nitrate hexahydrate [Ce(NO₃)₃⋅6H₂O] and cadmium chloride [CdCl₂] were used as source material. Concentrations were kept at 0.01 M. and mixed separately in distilled water for 10 minutes. Secondly, CeO₂ thin films with different Cd ratios (0, 10, 20, 30, 40, and 50 wt%) were deposited on the glass substrate at 300 ± 5°C. The starting solution was sprayed onto glass substrates for 20 minutes with an ultrasonic nozzle. Compressed ambient air was used to spray the prepared solution. the nozzle subtrate used was 30 cm. The solution flow rate was kept at 7.5 cc/min. Cd doped CeO₂ thin films were called the increasing Cd concentrations as CC0, CC10, CC20, CC30, CC40 and CC50, respectively.

The crystallization of the films have been identified by X-ray diffraction analysis (XRD) with a Panalitic Empyrian diffractometer using CuKα radiation. The optical analysis of films have been examined by UV–Visible spectrophotometer Shimadzu-Solid 2550. Photolumincense (PL) spectra has been studied Perkin Elmer LS55 with a xenon arc-lamp as the light source at 325 nm. Raman spectra has been recorded with a Renishaw in Via Raman microscope in the range 100–4000 cm^− 1. Surface images of the films have been studied by atomic force microscope (AFM) (Park Systems XE-100) with contact mode and the Hitachi Regulus 8230 scanning electron microscope (SEM) device. In addition, compositions have been investigated using SEM equipped for energy dispersive spectrometry (EDS) analysis.

3.1. Structural properties

XRD patterns of Cd doped CeO₂ films are shown in Fig. 2. All the diffraction peaks are seen in all the spectra, referred to cubic fluorite structure and matched with data available in ICDD (81–0792). No impurity peaks has been observed in all the films [27]. A decrease in the maximum intensity of the peaks is noticed with the addition of Cd. Because, the Ce^+ 3 with an ionic radius of 1.1 Å is larger than the Cd^+ 2 ion with an ionic radius of 0.97 Å. As the doping level increased, doping ions are occupied the intermediate sites. Crystallite size (D) of the films has been obtained from Scherrer’s equation;

where 0.9, contant value; λ, the wavelength of CuK_α radiation; β, the full width at the half-maximum of the peak and θ is the Bragg angle of the corresponding peak [28–31]. For the (2 0 0) peak that indicates the preferred orientation, the crystallite size of CC0 film has been calculated as 44 nm which gives information about the grain boundaries, defects, and also mechanical properties of crystals such as hardness or brittleness. The internal macro-stress or compaction due to doping, pressure and temperature effects during the formation of crystals is expressed as follows [32, 33].

$$<e>=(d- {d}_{0})/{d}_{0}$$

where d indicates the distance between the experimentally calculated crystal parallel planes corresponding to the peak (2 0 0) and d₀ shows the parallel inter planar distance in the absence of the standard distortion between the crystal planes given on the ICDD card. If the $e$values positive, there is macro strain; if negative, there is stress in the crystal structure. The intensity of linear defects (δ), especially in amorphous and polycrystalline structures, and the surface linear defect density (δ) have been calculated by Williamson and Smallman method using the following expression:

In crystal studies, n = 1 is generally taken. The linear defect density value is small and the degree of crystallization is good [34, 35].

Table 1

Some data of Cd doped CeO₂ films obtained from XRD pattern.
Film	2θ(°)	d(Å)	2θ₀(°) (ICDD)	d₀(Å) (ICDD)	(h k l)
CC0	29.03	3.074	28.55	3.124	(1 1 1)
	33.69	2.658	33.08	2.706	(2 0 0)
	48.09	1.891	47.49	1.913	(2 2 0)
	59.49	1.553	59.10	1.562	(2 2 2)
	69.91	1.356	69.42	1.353	(4 0 0)
CC10	28.99	3.078	28.56	3.124	(1 1 1)
	33.53	2.673	33.08	2.706	(2 0 0)
	48.08	1.892	47.49	1.913	(2 2 0)
	59.68	1.549	59.10	1.562	(2 2 2)
	69.62	1.351	69.42	1.353	(4 0 0)
CC20	29.19	3.059	28.55	3.124	(1 1 1)
	33.61	2.667	33.08	2.706	(2 0 0)
	48.26	1.886	47.49	1.913	(2 2 0)
	59.88	1.545	59.10	1.562	(2 2 2)
	69.95	1.344	69.42	1.353	(4 0 0)
CC30	29.22	3.057	28.55	3.124	(1 1 1)
	33.58	2.667	33.08	2.706	(2 0 0)
	48.33	1.883	47.49	1.913	(2 2 0)
	56.98	1.616	56.35	1.632	(3 1 1)
	70.08	1.343	69.42	1.353	(4 0 0)
CC40	29.24	3.054	28.55	3.124	(1 1 1)
	33.72	2.658	33.08	2.706	(2 0 0)
	48.17	1.889	47.49	1.913	(2 2 0)
	60.03	1.541	59.10	1.562	(2 2 2)
	70.24	1.339	69.42	1.353	(4 0 0)
CC50	29.24	3.054	28.55	3.124	(1 1 1)
	33.56	2.671	33.08	2.706	(2 0 0)
	48.09	1.892	47.49	1.913	(2 2 0)
	59.45	1.555	59.10	1.562	(2 2 2)
	69.81	1.347	69.42	1.353	(4 0 0)

Table 2

Structural parameters of Cd doped CeO₂ films.
Film	β(°)	D (nm)	<e>	δ (1/nm²)
CC0	0.187	44	-0.0177	5.17x10^− 4
CC10	0.064	130	-0.0122	5.92x10^− 5
CC20	0.048	180	-0.0144	3.46x10^− 3
CC30	0.078	81	-0.0144	1.52x10^− 4
CC40	0.089	93	-0.0177	1.16x10^− 4
CC50	0.089	93	-0.0129	1.16x10^− 4

3.2. Optical properties

Figure 3 indicates the tranmittance spectra of the films between the 300–900 nm wavelengths. It is clear from these spectra that film presents the increasing absorbance values between the 375–400 nm that indicates the optical band edges of the CeO₂ film. Optical band gap energy (E_g) of the films has been calculated by optical method using (αhν)²∼ (hν) plot and shown in Fig. 4.

(αhυ) = A(hυ-E_g)ⁿ

In where, A is a constant, α (in cm^− 1) is the linear absorption coefficient, and hυ is the energy of incident photons. As for the exponent, the value of n depends upon the type of the transition that may have values 1⁄2 and 2 corresponding to the allowed direct and indirect transitions [36–39]. Since these films have a direct band structure, n was taken to be 1⁄2 for the allowed direct transition.

The plot of (αhν)² vs hν is displayed in the inset of Fig. 4. E_g values of the Cd doped CeO₂ films are in the range of 3.23–3.52 eV, and are higher than of the bulk CeO₂ (3.2 eV) [40, 41].

PL spectroscopy is a rapid and non-limiting technique for the determining the optical properties like defect levels of semiconductor crystals [42]. Figure 5 shows PL spectra in the 400–800 nm wavelength range and 380 nm excitation wavelength to determine this behavior of Cd doped CeO₂ films. PL emissionis observed from violet to red region. Additionally, many shoulder peaks are located in the blue region due to surface-related defects, while other peaks are due to dislocations or oxygen vacancies. It can be seen that the PL intensity of Cd doped CeO₂ is lower than that of undoped CeO₂. An green emission band is due to the transition from the Cd donor level to the oxygen vacancies level localized in the CeO₂ band gap [43, 44]. Since Ce^+ 4 and Cd^+ 2 have different covalent and ionic radii, it is thought that replacing Ce with Cd will create oxygen vacancies (V_o⁺⁺) to maintain neutrality [27, 37]. CeO₂ show outstanding catalytic activity in most of the chemical reactions, for properties oxygen storage capacity, that readily changes between Ce^+ 3 and Ce^+ 4 states. In addition, there are many overhanging bonds and defects on the surface of CeO₂ films [40]. Kumar et al. [41] have stated that as the O^− 2/O⁻ surface system is the trap of the holes in the valence band of doped CeO₂ plays role in the formation of visible emission centers (V_o⁺⁺) [42–45].

Raman spectra of Cd doped CeO₂ films as shown in Fig. 6. Raman spectra show the second order transverse acoustic (2TA) modes at ~ 250 cm^− 1, a defect-induced (2TO) mode at ~ 600 cm^− 1, and the second order longitudinal optical mode (2LO) at ~ 1170 cm^− 1 [45–48]. Also, there is an intense peak at 461 cm^− 1, which related to the F_2g symmetrical mode of the fluorite structure [45, 46]. The peak at 570 cm^− 1 related to the LO mode of fluorite-structured cerium oxide materials, that is, to the oxygen vacancy (V_o) defects in the structure [47, 48].

3.3. Surface properties

SEM images of Cd doped CeO₂ films are showed Fig. 7. Generally, morphology of Cd doped CeO₂ films can be classified into three structures: small dots in whitish color, large bright plates, and matrix that spreads over the surface in pale colored regions. SEM image corresponding to the element mapping images of Ce, O and Cd elements distributed uniformly within the composites is given Fig. 8. The elemental composition of the films is carried out by EDX method, and the data are also given in Table 3. According to the EDS spectrum, the cerium atoms in the sprayed CeO₂ film have been determined as more dominant than oxygen in percentage.

Table 3

Compositional analysis of Cd doped CeO₂ films.
Film	CC0	CC10	CC20	CC30	CC40	CC50
Wt (%) O	20	27	21	25	37	32
Wt (%) Cd	0	10	15	18	28	31
Wt (%) Ce	80	63	64	57	35	37

Cd doped CeO₂ films that are used as anti-reflective layers on solar cells should have suitable surface roughness and should pass the sunlight to the absorber layer of the solar cell as much as possible. Because each photon absorbed by the absorber layer forms an electron-hole pair hindrance to the passage of photons by the anti-reflective layer will lower the efficiency of the cell. So that, the AFM images are utilized to examine the atomic (grain) aggregates on the resulting sprayed film surface and given in Fig. 9. The sprayed films are formed on glass substrates, and surface morphology of the crystal structure cannot be homogeneous because the surface of the glass substrates which has defects due to missing chemical bonds. Even if the formation of Cd doped CeO₂ films is weak, the grown crystal structure tends to follow the crystal structure of the substrate. The hills and valleys in the 3D AFM image of the sprayed CeO₂ films are formed as a result of different atomic stacks. The appearance of white hills also could be attributed to the accumulation of excess atomic clusters in these regions which causes the thinner film formation in the valleys. The thermal shock effect and the spray cones are more likely to form these valleys.

Table 4

Roughness values of Cd doped CeO₂ films.
Film	CC0	CC10	CC20	CC30	CC40	CC50
R_pv (nm)	485	300	149	193	326	541
R_q (nm)	58	22	20	31	36	61
R_a (nm)	45	15	16	25	29	47

3.4. Photodegradation of the Cd doped CeO₂ films

Methyl orange is a real pH indicator. It is an organic substance that changes color depending on the pH of the environment. In an acidic medium, methyl orange is red, while in an alkaline medium, its color turns yellow. In addition, methyl orange, a colored organic substance, is in the azo dye (–N = N–) class. In addition, dyestuffs in this class are also defined as pollutants due to their negative effects on human and environmental health [49]. Therefore, such substances need to be removed or even destroyed from environmental and food samples.

The photodegradation technique is the simplest, fastest, most economical, and environmentally friendly for the removal of pollutants. Therefore, the capacitance of Cd doped CeO₂ thin films produced in different components for the removal of the methyl orange as a indicator was investigated under UV light. Therefore, first of all, standard methyl orange solutions were prepared precisely and a calibration chart was created in Fig. 10 scanning the overall absorbance of the UV-Vis spectrophotometer from 300 to 800 nm.

For the methyl orange removal study, it has been first kept in thin films for 30 minutes in a dark environment. Then, it has been kept under UV light for about 6 hours and the absorbance of the solution has been measured with a UV-vis spectrophotometer for each 30 minutes. At the end of 6 hours, the capacities and kinetic models of Cd doped CeO2 films used in the removal of methyl orange have been explained. The performance of the photocatalyst in the degradation of organic dyes with CeO2:Cd catalyst has been determined by the degradation rate of the dye, known as the kinetic data. These models have been based on the Langmuir- Hinshelwood kinetic equation:

$$-\text{ln}\left(\frac{C}{{C}_{0}}\right)=kt$$

According to the equation, the time-dependent ln(C/C₀) graph can be drawn and the photocatalytic rate constant (k) value can be calculated from the slope of this graph [50, 51].

The changes in concentration, percent degradation, and the time-dependent ln(C_0/C) curves for the methylene orange solution as a function of irradiation time for CeO₂:Cd films are shown in Fig. 11 (a, b, and c), respectively. The initial concentration of methylene orange is C₀ = 4x10^− 4mgL^− 1 as shown in Fig. 11 (a). There are some important issues when studying the photocatalytic reaction. Examples include the absorption of light by a semiconductor to form electron-hole pairs, charge separation and transport to the surface of the semiconductor, and reactant adsorption and surface reactions. Studying the light absorption properties of materials is crucial in the context of photocatalysis because it helps determine the efficiency of a photocatalyst in harnessing light energy to drive chemical reactions. Before investigating the photocatalytic performance of the samples, the light absorption property of Cd doped CeO₂ photocatalysts is studied by UV–Vis the absorption spectra shown in Fig. 4. It can be seen Fig. 4, Cd doping clearly impress light absorption characteristics of CeO₂. When the XRD patterns are examined and the crystallinity value is calculated in Table 2 it is observed that the grain size increases with the amount of additive. Although the grain size increases, it shows that the deformation of the crystal is low with small macrostrain values. According to AFM images, there are formations like building blocks formed on the surfaces of Cd doped CeO₂ films. Together with higher RPV roughness values, it may cause better adhesion of methylene orange to the film surface. Such an effect may be due to defects that restrict the recombination of electron–hole pairs along with the Cd doping. Increasing the defect states for Cd doped CeO₂ films may cause more carriers to be transferred to the film surface and dye molecules may cause the Cd doped CeO₂ films to react [52]. Dye molecules adsorb on the photocatalysis surface. Degradation of organic pollutant is an important process.In addition, the surface texture of Cd-doped CeO₂ films (micro-sized block structures and valleys consisting of nano-sized particles) is of great importance.

In the current work, the Cd doped CeO₂ films have been obtained by USP technique onto Pyrex glasses at 300 ± 5°C substrate temperature. Therefore, it turns out that each variable has a significant effect on the properties of optoelectronic devices, demonstrating that detailed investigations are still necessary. At the same time, The effect of photoactivity on the films was investigated by using methylene orange organic pollutants. All the films exhibit single-phase crystalline and cubic fluorite structures with preferred orientation along (2 0 0) direction. PL spectra revealed the presence of emission peaks centered at 530 and 600 nm in the visible region. In the transmission spectra, the Cd doped CeO₂ films is presented at 60% transparency in the wavelength range from 300 to 700 nm of the visible region. An optical bandgap of 3.52 eV is obtained for the prepared film. When the crystallization levels are examined, it is observed that the active surface area is formed and they are suitable candidates for photocatalytic applications. The degradation percentages of the films vary in the range of 75–78. It is concluded that all films are suitable for photocatalytic applications in the environmental and energy fields.

Ethical Approval

The study is not a article of humans or animals. Ethical approval is not required.

Funding

No financial support was received.

Availability of data and materials

No, I don't have any research data outside the submitted manuscript file.

Author Contribution

Author contributions ED contributed to conceptualization, review & editing;MSC contributed to, project administration and supervision.SK contributed to investigation, visualization, writing theoriginal draft; ED contributed to data curation, and MSC and SK contributed to formal analysis; All authors have read and agreedto the published version of the manuscript.

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No competing interests reported.

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Developed and characterization of a novel Cd doped CeO₂ nanofilm and application of pesticide removed by photodegradation

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental details

3. Results and discussion

3.1. Structural properties

3.2. Optical properties

3.3. Surface properties

3.4. Photodegradation of the Cd doped CeO₂ films

4. Conclusion

Declarations

References

Additional Declarations

Status:

Version 1

Developed and characterization of a novel Cd doped CeO2 nanofilm and application of pesticide removed by photodegradation

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental details

3. Results and discussion

3.1. Structural properties

3.2. Optical properties

3.3. Surface properties

3.4. Photodegradation of the Cd doped CeO2 films

4. Conclusion

Declarations

References

Additional Declarations

Status:

Version 1

Developed and characterization of a novel Cd doped CeO₂ nanofilm and application of pesticide removed by photodegradation

3.4. Photodegradation of the Cd doped CeO₂ films