Physiochemical, radiative transitions and thermoluminescence characterizations of nano Ce-doped monoclinic barium titanate

doi:10.21203/rs.3.rs-5218309/v1

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Physiochemical, radiative transitions and thermoluminescence characterizations of nano Ce-doped monoclinic barium titanate

https://doi.org/10.21203/rs.3.rs-5218309/v1

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This article reports the preparation, analytical, and thermoluminescence (TL) characterization of BaTi₅O₁₁ doped with different concentrations of Ce. The Sol-gel technique was used to synthesize the doped nanocrystals. The prepared samples were examined by XRD, EDX, UV-V_is spectrophotometry, SEM, and TEM techniques to determine their analytical features. The samples with 0.7% Ce doping showed the highest TL sensitivity for ionizing radiation among the samples prepared with different concentrations. The glow curves analysis showed that there were seven peaks that overlapped with each other with thermal activation energies: 0.93, 1.08, 1.16, 1.23, 1.29, 1.35, and 1.38 eV. The dose-response linearity and reusability measurements displayed that 0.7% Ce-doped BaTi₅O₁₁ can be used in monitoring high doses radiation applications.

Sol-gel method

Thermoluminescence

Kinetic parameters

Beta dosimetry

Ce dopant

When a solid material gets radiation and then heat, it gives off light (or luminescence). This is called thermoluminescence (TL) [1]. The TL technique has many applications, like dating [2, 3] and dosimetry [4, 5], but it can also be used in material science for its accurate results in characterizing the existence of defects and in determining their location within the band gap. These defects may be naturally present in the material or created by doping the material of interest [6]. We use the TL technique to explain how luminescence works and to study the behavior of the charged carriers that cause the TL. The TL technique was used to examine various materials to measure and describe their kinetic features, like how deep the traps are (E), how the traps change (b), and how likely the traps are to release the charges (s) [7–10].

Besides the study and investigation of natural and artificial bulk materials, metal oxide nanoparticles were also studied for various purposes such as radiation dosimetry, purification systems, optical devices, photovoltaics, photocatalysis…etc. [11–14]. The reason for such interest in metal oxides is their novel and unique properties such as electrical conductivity, light emission, chemical reactivity, active surface, and hardness [15, 16]. In the last decays, many studies work on improving the properties of metal oxides by doping [17, 18].

Previous work reported that they made inorganic phosphors with rare earth doping, such as borates, silicate, aluminates, oxides, and titanates that had different properties. They used various methods to make them, such as combustion, Sol-gel, co-precipitation, solid state synthesis and so on [19–22].

Rare earth metals (REM) have special 4f-electron properties that enable their use in modern phosphors, catalysts, and magnets [23–26]. Being one of the most abundant REM, cerium has versatile features such as rich oxidation-reduction properties, adaptable coordination capacity, and high electron transport [27–29]. It has been proven by many experiments that the speed of electron-hole rejoining can be decreased by adding suitable rare earth ions (especially Ce and La) as dopants [30–33]. Moreover, adding cerium to metal oxide can form defect energy levels inside the band gap, which can affect the properties related to light and electricity, as observed in Ce-TiO₂ [34], Ce-ZnO [35], and Ce-SnO₂ [36].

BaTi₅O₁₁ has a high dielectric constant and a low dielectric loss, which makes it suitable for capacitors, sensors, and actuators. In addition, BaTi₅O₁₁ exhibits ferroelectric and piezoelectric behaviors, which means that it can change its polarization and shape in response to electric fields and mechanical stresses, respectively. These behaviors can be used for memory devices, energy harvesting, and transducers. Besides all of that, there has been no one who has studied the ability to study the thermoluminescence characteristics of this material before. Consequently, the current study focuses on preparing BaTi₅O₁₁ samples doped with various amounts of cerium; the X-ray diffraction (XRD) analysis is utilized to show the shape of the crystals in the samples. Beta radiation is employed to measure the Thermoluminescence (TL) response and determine the kinetic parameters. X-ray Photoelectron Spectroscopy (XPS), scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) methods are employed to explore the chemical composition and appearance of the samples.

2.1. Materials and method of preparation

A series of BaTi₅O₁₁ with 0.3%, 0.5%, 0.7%, and 1% Ce doping were prepared using the Sol-gel technique, which is displayed in Fig. 1. Cerium (Ⅲ) nitrate hexahydrate [Ce(NO₃)₃.6H₂O; Aldrich], barium acetate [Ba(CH₃COO)₂], Aldrich), and Titanium isopropoxide [Ti(OCH(CH₃)₂)]₄, Aldrich), were used as precursors. To prepare 0.3% Ce- doped BaTi₅O₁₁, 2.3037 g of barium acetate and 0.0117 g of Cerium (III) nitrate hexahydrate were dissolved separately in acetic acid at 50 ℃, with continuous stirring. Then 13.5 ml of titanium isopropoxide was mixed with ethanol, with continuous stirring. The solution of titanium isopropoxide was stirred constantly as the solutions of barium acetate and cerium nitrate were poured in, one by one. The gel was formed by adding ammonium hydroxide (NH₄OH, 1M) dropwise to the solution while stirring. The gel was rinsed with distilled water and filtered, then heated for 12 hours at 80 ⁰C to dry. The material was ground to fine powder by using a pestle and mortar and then calcinated for 2 hours at 800 ⁰C. The same method was used to synthesis the rest of the Ce-doped BaTi₅O₁₁ samples. The samples were labeled as C0.3%, C0.5%, C0.7%, and C1.0%.

2.2. Material characterization

The samples’ crystallinity and phase identification were found out by using a Bruker-D8 Discover (Germany) XRD. The XRD measurements were performed at room temperature using an X-Ray copper tube (CuKα) as a source of radiation with wavelength = 1.54 ̊A. The current and voltage of the diffractometer were 40 mA and 40 kV, respectively. The crystalline phase was identified by comparing the obtained XRD patterns with the JCPDS diffraction data cards.

The TL characteristics were studied by using a luminescent reader called Lexsyg Smart TL/OSL (Germany). LexStudio 2.0 operating software is used to operate the reader. The device had a ⁹⁰S/⁹⁰Y source that gave out β-particles with a top energy of 2.2 MeV and irradiated at 0.11 Gy/s. It also contained a Hamamatsu bi-alkaline cathode photomultiplier tube. The IRSL/TL – wideband blue optical window was utilized to record the TL readings.

UV − Vis spectrophotometer (UV-2600, Japan) was utilized to determine the band gap of the samples. The Thermo Scientific-K-Alpha XPS device (USA) was utilized to study the elemental composition and chemical state of the atoms in the material and to chemically analyze the prepared samples. SEM with EDX (ZEISS-EVO 15, Germany) was used to examine the shape of the prepared powder more closely and find out the elemental composition of a chosen samples. The particle shape and size of the samples of interest were also examined by using JEOL JEM-2100 TEM (Japan).

3.1. X-Ray Diffraction (XRD)

Figure 2 shows the XRD spectra of the BaTi₅O₁₁ with Ce doping samples. The standard monoclinic BaTi₅O₁₁ of JCPDS card no. 35–0805 matches all the diffraction peaks. The enlarged (140) crystal plane diffraction peaks shift to larger angles. This distortion in crystallinity is due to the replacement of Ba²⁺ (1.35 ⁰A) [37] with Ce³⁺ (1.143⁰A) [38] where the smaller radii ions would replace the larger ones.

3.2. Crystal structure of C0.7% samples from XRD

The peak position, Miller indices, and d-spacing of the C0.7% samples are listed in Table 2. The following equation can be used to calculate the lattice parameters a, b, and c for C0.7% monoclinic samples [39].

$$\:\frac{{\varvec{s}\varvec{i}\varvec{n}}^{2}\left(\varvec{\beta\:}\right)}{{\varvec{d}}_{\varvec{h}\varvec{k}\varvec{l}}^{2}}\:=\:\frac{{\varvec{h}}^{2}}{{\varvec{a}}^{2}}+\:\frac{{\varvec{K}}^{2}\:{\varvec{s}\varvec{i}\varvec{n}}^{2}\left(\varvec{\beta\:}\right)}{{\varvec{b}}^{2}}+\:\frac{{\varvec{l}}^{2}}{{\varvec{c}}^{2}}-\:\frac{2\varvec{h}\varvec{l}\:\varvec{c}\varvec{o}\varvec{s}\:\varvec{\beta\:}}{\varvec{a}\varvec{c}}$$

For (022) d₀₂₂ = 3.2408

$$\:\frac{{sin}^{2}\left(\beta\:\right)}{{3.2408}^{2}}\:=\:\frac{{4c}^{2}{sin}^{2}\left(\beta\:\right)+{4b}^{2}}{{b}^{2}{c}^{2}}$$

For (023) d₀₂₃ = 2.304

$$\:\frac{{sin}^{2}\left(\beta\:\right)}{{2.304}^{2}}\:=\:\frac{{4c}^{2}{sin}^{2}\left(\beta\:\right)+{9b}^{2}}{{b}^{2}{c}^{2}}$$

(Eq. 1) ÷ (Eq. 2)

$$\:{c}^{2}{sin}^{2}\left(\beta\:\right)\:=\:0.27744\:{b}^{2}$$

For (002) d₀₀₂ = 3.674

$\:{c}^{2}{sin}^{2}\left(\beta\:\right)$ = 54.01368 (4)

Substituting the value of $\:{c}^{2}{sin}^{2}\left(ꞵ\right)$ of Eq. (4) in Eq. (3) yields

b = 13.95 ⁰A

By the same way a = 7.544 ⁰A, and c = 7.452 ⁰A.

The most intense peak (1 4 0) at 2θ = 28.5⁰ was considered for the determination of β_hkl [40, 41]. The FWHM of the XRD was obtained by using Origin Pro 2018 and was also used to calculate the crystallite size according to Scherrer’s equation [42] given by:

D = $\:\frac{\varvec{K}\:\varvec{\lambda\:}}{{\varvec{\beta\:}}_{\varvec{h}\varvec{k}\varvec{l}\:}\varvec{C}\varvec{o}\varvec{s}\:\varvec{\theta\:}}$ (5)

Where k is a shape factor (0.9), λ is the wavelength of CuKα radiation (0.1544 nm), ꞵ_hkl is full width at half maximum (FWHM) in radians, and θ the Bragg's angle in radians. From the calculations, the crystallite size obtained for the C0.7% samples were found to be 29.37 nm.

D = $\:\frac{\varvec{K}\:\varvec{\lambda\:}}{{\varvec{ꞵ}}_{\varvec{h}\varvec{k}\varvec{l}\:}\varvec{C}\varvec{o}\varvec{s}\varvec{\theta\:}}$ (6)

Where λ is the wavelength of CuKα radiation (0.1544 nm), βhkl is full width at half maximum (FWHM) in radians, and θ the Bragg's angle in radians. The shape factor (K) is a parameter that depends on the crystal structure. For cubic or rhombus-shaped crystallites, K can be assumed to be 0.94 or 0.89, respectively. However, these values may not be accurate for monoclinic crystallites, which may have different degrees of elongation or asymmetry. Therefore, we used 0.9 as a reasonable approximation [43]. From the calculations, the crystallite size obtained for the C0.7% samples were found to be 29.37 nm.

Table 1

The XRD peaks’ position, Miller indices, and d-spacing of the C0.7% samples.
2θ (Degree)	Miller indices (hkl)	d-spacing (⁰A)	2θ (Degree)	Miller indices (hkl)	d- spacing (⁰A)
15.8	(-101)	5.590	36.3	(-241)	2.468
17.7	(120)	5.001	39.05	(023)	2.304
22.9	(031)	3.877	41.6	(232)	2.166
23.9	(200)	3.707	43.2	(161)	2.092
24.2	(002)	3.674	44.8	(-341)	2.019
26.3	(-112)	3.382	46.7	(-171)	1.943
27.2	(220)	3.267	49.5	(-153)	1.837
27.5	(022)	3.2408	52.6	(-262)	1.737
28.5	(140)	3.121	54.2	(262)	1.688
30.3	(-141)	2.943	56.6	(361)	1.623
31.1	(221)	2.867	59.7	(073)	1.547
31.9	(122)	2.795	63.1	(-363)	1.471
34.3	(231)	2.608	65.2	(380)	1.428

3.3. X-ray photoelectron spectroscopy (XPS)

We used the XPS technique to examine the elemental composition of C0.7% samples. The survey spectrum in Fig. 3a indicates that high-resolution spectra of Ce 3d, Ba 3d, Ti 2p, and O 1s photoelectron peaks are detected. It is known that the line shapes of Ce⁴⁺ and Ce³⁺ are not the same, and this makes the spectra of cerium very complicated, especially when both forms are there. Ce⁴⁺ has a prominent peak near 916 eV that is absent in Ce³⁺ [44]. As seen in Fig. 3b, the Binding energy of Ce 3d5/2 is 886.83 eV and the binding energy of Ce 3d3/2 is 899.97 eV, and a band shape characteristic for Ce³⁺. The absence of strong peaks around 916 eV ruled out the presence of Ce⁴⁺ ions.

3.4. Energy dispersive X-Ray spectroscopy (EDX) and scanning electron microscopy (SEM)

Figure 4a, b show the EDX data of the C0.7% samples. The spectrum analysis verifies the presence of Ba, Ti, Ce, and O in the prepared samples and provides the corresponding weight % and atomic %. The SEM technique was applied to study the surface morphology of the C0.7% samples. The formation of quasi-spherical nanoparticles with varying particle sizes was observed in Fig. 4c, d.

3.5. Transmission Electron Microscope (TEM)

The particle size distribution and morphology of the C0.7% samples were studied by using TEM. The analysis of the measured data confirmed that the powder particles are quasi-spherical nanoparticles, shown in Fig. 5a. The SAED pattern in Fig. 5b yielded a set of rings with spots suggesting that nanoparticles have a large grain size. The histogram in Fig. 5c shows that the particle size of the C0.7% samples mostly varies between 31 and 106 nm. The average particle size is calculated to be 73 nm.

3.6. Results of Thermoluminescence (TL)

3.6.1. TL-Glow Curve

The TL glow curves and TL response (indicated by the total area under the glow curve) of the Ce-doped BaTi₅O₁₁ samples after exposure to a ꞵ-dose of 55 Gy are shown in Fig. 6. The glow curves and TL-intensity, that are shown, physically correspond to the energy that the material stores and emits when it is exposed to radiation and heat, respectively [45]. Figure 6 shows a wide glow peak at about 335 K, which indicates that the glow curves have several TL glow peaks that overlap. A carrier trap, which is a localized state in the band gap between the conduction band minimum (CBM) and the valence band maximum (VBM), corresponds to each glow peak. The TL response was the highest for the C0.7% samples. Therefore, the properties of this specific concentration will be the focus of the following sections.

3.6.2. Kinetic parameters

The kinetic parameters and number of the carrier traps in the C0.7% samples were estimated by using experimental and computational methods. The number and positions of the overlapping peaks that form the glow curves were estimated by using the T_max-T_stop method as an experimental method. The peaks that compose the glow curves were analyzed for their kinetic parameters simultaneously by using Glow Curve Deconvolution software.

3.6.2.1. T_max-T_stop method

This method involves many steps illustrated as follows [46]:

Exposing the prepared samples to an arbitrary dose of radiation (chosen to be 55 Gy).

Raising the samples’ temperature from room temperature to a temperature that matches the initial rise of the displayed glow curves (323 K for the first cycle), which is named T_stop (First TL measurement).

Bringing the heated samples back to room temperature by cooling it down.

The temperature corresponding to the first maximum intensity in the TL glow curve of the cooled samples (second TL reading) was measured. This temperature is known as T_max.

Repeating the previous four steps with increasing T_stop with a temperature step of 5 K each cycle.

Finally, plotting the values of T_max against those of T_stop, which results in a staircase-like curve indicating an estimate of how many overlapping peaks made up the glow curve.

In the current measurements, the T_stop was raised from room temperature to 460 K and every cycle the value of T_max was recorded. Figure 7 shows the plateau of T_max vs. T_stop of the C0.7% samples from which 7 overlapping peaks can be identified. Consequently, we used the computational glow curve deconvolution method to get the kinetic parameters of seven TL glow peaks that were assumed to compose the TL glow curves. The results revealed that P1, P4, P6 and P7 are localized energy traps with constant Tm’s and P2, P3 and P5 are energy distribution of electron trap centers.

3.6.2.2. Glow Curve Deconvolution (GCD)

El-Kinawy et al. [47] used private TL software to perform the GCD. As shown in Fig. 8, the GCD method separated the glow curve into its TL components. The lower part of Fig. 8 shows the residue, which is the difference between the fitted and experimental curves. The FOM value indicates how well the fitted curve matches the experimental curve. As seen in Table 1, The FOM value, which is below 1%, shows how good the fit is to the data. The Calculated kinetic parameters: namely, the attempt-to-escape factor s (s^− 1), trap center position T_M (K), kinetic order b, and trap depth E (eV) are summarized in Table 2 including the standard errors of all kinetic parameters. The values of the trap depths were found to lie within the range of 0.93–1.38 eV. It was found that the TL glow peaks are located at 384.27, 409.69, 432.81, 460.77, 594.78, 536.99, and 586.49 K, respectively. According to the results, the attempt-to-escape factor values are of the order of lattice vibrations: namely, on the order or 11^− 13 s^− 1. The order of kinetics values was around: 1.44, 1.36, 1.50, 1.47, 1.56, 1.60, and 1.50. All peaks show general order kinetics based on the values of b.

Table 2

Kinetic parameters of the C0.7% samples obtained by using GCD.
Peak	E (eV)	T_M (k)	s (s^− 1) x10¹²	b	FOM (%)
1	0.93 ± 0.006	384.27 ± 2.60	0.59 ± 0.004	1.436 ± 0.010	0.94
2	1.08 ± 0.007	409.69 ± 2.44	8.0 ± 0.048	1.363 ± 0.008
3	1.16 ± 0.0062	432.81 ± 2.31	13.0 ± 0.069	1.501 ± 0.008
4	1.23 ± 0.0029	460.77 ± 1.09	11.1 ± 0.026	1.467 ± 0.003
5	1.29 ± 0.0026	494.78 ± 1.01	4.6 ± 0.009	1.563 ± 0.003
6	1.35 ± 0.0023	536.99 ± 0.93	1.5 ± 0.003	1.598 ± 0.003
7	1.38 ± 0.0020	586.49 ± 0.85	0.19 ± 0.001	1.503 ± 0.002

3.6.3. Dose-response linearity

The C0.7% samples were irradiated to ꞵ-rays at doses from 5.5 Gy to 385 Gy and its output TL light was recorded to study the response behavior of the prepared samples under investigation. A wide band blue detection window which consists of a filter combination of “Schott KG 3 + Schott BG 25” was utilized to read the glow curves. The glow curves of the samples after irradiation are shown in Fig. 9a. The inset in Fig. 9a displays the dose-response of the whole glow curves to the radiation dose applied. The inset shows that the glow curves are dose-dependent in the range of 5.5 Gy – 275 Gy after which the glow curves display a supralinear behavior.

The dose-response characteristic of the C0.7% samples was fully described by separating the observed glow curves and studying how each peak responds to the dose. Figure 9b displays the area under each TL glow peak. The fitting of the area under each TL glow peak revealed that peaks 2–7 had a proportional response to the radiation applied in the dose range from 5.5 Gy to 385 Gy. However, a power function of the form a*x^(b), where a & b are fitting parameters, and (x) is the applied dose, was used to fit the area below peak 1. The figure demonstrates that the area under the TL peak 1 began to show a flattening trend after the dose of 275 Gy.

3.6.4. Reusability

To test the repeatability using the prepared samples to display the same TL response when irradiated to the same applied dose, the C0.7% samples were exposed to β-rays (55 Gy) and the glow curves were read six times. The glow curves were then separated into their individual glow peaks. Figure 10 shows the area below each glow peak for each reading cycle. The plots of total area below the glow peaks confirms the reliability to reuse the C0.7% samples for radiation dosimetry.

3.7. UV − Vis diffuse reflectance spectrophotometer (DRS)

Figure 11a displays the DRS spectrum of C0.7% samples in the wavelength range of 200–800 nm. The Tauc relation [48] is used to calculate the band gap (Eg) from the DRS spectrum.

αhυ = C (hυ-Eg)ⁿ (7)

where C is a constant, α is the molar absorption coefficient, hυ is the photon energy, and n is the exponent that indicates the type of electronic transition (for direct transition n = 1/2) [49]. The value of the Eg of C0.7% samples has been determined to be 3.37 eV (Fig. 11b).

If the radiative transitions of the luminescence process were supposed to occur from the non-localized conduction band, a simplified band diagram of the host C0.7% samples with the seven carrier traps can be drawn, presented in Fig. 12. The charge carrier levels are located at 0.93, 1.01, 1.16, 1.23, 1.29, 1.35, and 1.38 eV below the level of the conduction band which set to 3.37 eV (from Fig. 11b). The valence band maximum was set to zero.

The Sol-gel method is used to prepare Ce-doped BaTi₅O₁₁ samples. The defect characteristics, morphology, and crystal structure of the samples were studied by using different experimental and computational methods. The same diffraction peaks that matched the monoclinic structure were shown by the XRD spectra of the samples with dopants. The TL technique was used to study the existence of defects in the prepared samples and to test the dosimetric properties to beta radiation. The C0.7% samples has shown the highest TL response when exposed to ꞵ-radiation of 55 Gy. The C0.7% samples has shown a proportional dose-response in the range of 5.5 Gy − 385 Gy. The samples also displayed good repeatability when irradiated with 55 Gy of ꞵ-dose six times. The analyses of the SEM and TEM data indicated that C0.7% samples had uniform quasi-spherical particles with an average size of 73 nm. The calculated effective atomic number of the compound was 24.04. These all characteristics confirmed that 0.7% Ce-doped BaTi₅O₁₁ can be used in monitoring high doses radiation such as detection inside nuclear reactors, during food sterilization and materials testing.

Conflict of interest

No conflict of interest

Acknowledgment

The authors acknowledges that the current work was personally financed.

Ethical approval:

The authors declare that the current study didn’t carry out experiments involving human tissue.

Authors Contributions:

Ghada Bassioni: Conception, experimental design and manuscript composition.

Mohamed El-Kinawy: Carrying out measurements and writing.

Manar Mostafa: Carrying out measurements, writing.

Nabil El-Faramawy: Conception, experimental design, writing and manuscript composition.

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You are reading this latest preprint version

Physiochemical, radiative transitions and thermoluminescence characterizations of nano Ce-doped monoclinic barium titanate

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials and method of preparation

2.2. Material characterization

3. Results and discussions

3.1. X-Ray Diffraction (XRD)

3.2. Crystal structure of C0.7% samples from XRD

3.3. X-ray photoelectron spectroscopy (XPS)

3.4. Energy dispersive X-Ray spectroscopy (EDX) and scanning electron microscopy (SEM)

3.5. Transmission Electron Microscope (TEM)

3.6. Results of Thermoluminescence (TL)

3.6.1. TL-Glow Curve

3.6.2. Kinetic parameters

3.6.2.1. T_max-T_stop method

3.6.2.2. Glow Curve Deconvolution (GCD)

3.6.3. Dose-response linearity

3.6.4. Reusability

3.7. UV − Vis diffuse reflectance spectrophotometer (DRS)

4. Conclusions

Declarations

References

Additional Declarations

Status:

Version 1

Physiochemical, radiative transitions and thermoluminescence characterizations of nano Ce-doped monoclinic barium titanate

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials and method of preparation

2.2. Material characterization

3. Results and discussions

3.1. X-Ray Diffraction (XRD)

3.2. Crystal structure of C0.7% samples from XRD

3.3. X-ray photoelectron spectroscopy (XPS)

3.4. Energy dispersive X-Ray spectroscopy (EDX) and scanning electron microscopy (SEM)

3.5. Transmission Electron Microscope (TEM)

3.6. Results of Thermoluminescence (TL)

3.6.1. TL-Glow Curve

3.6.2. Kinetic parameters

3.6.2.1. Tmax-Tstop method

3.6.2.2. Glow Curve Deconvolution (GCD)

3.6.3. Dose-response linearity

3.6.4. Reusability

3.7. UV − Vis diffuse reflectance spectrophotometer (DRS)

4. Conclusions

Declarations

References

Additional Declarations

Status:

Version 1

3.6.2.1. T_max-T_stop method