Effect of Laser Heating on Partial Decomposition of Bi<sub>12</sub>SiO<sub>20</sub> (BSO) Single Crystal: Raman Study

Romcevic, Nebojsa; Hadzic, Branka; Prekajski Đorđević, Marija; Mihailovic, Peda; Curcic, Milica; Trajic, Jelena; Mitric, Jelena; Romcevic, Maja

doi:https://doi.org/10.1155/2023/5490018

Journal of Spectroscopy

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Abstract Introduction Materials and Methods Results Discussion Conclusion Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 5490018 | https://doi.org/10.1155/2023/5490018

Effect of Laser Heating on Partial Decomposition of Bi₁₂SiO₂₀ (BSO) Single Crystal: Raman Study

Nebojsa Romcevic,¹Branka Hadzic,¹Marija Prekajski Đorđević,²Peda Mihailovic,³Milica Curcic,¹Jelena Trajic,¹Jelena Mitric,¹and Maja Romcevic¹

Academic Editor: Emiliano Bonera

Received02 Mar 2023

Revised17 Apr 2023

Accepted28 Apr 2023

Published04 May 2023

Abstract

The effect of laser (532 nm line of Verdi G) heating during the Raman measurements, on partial decomposition of Bi₁₂SiO₂₀ single crystal, was addressed in this study. The degree of decomposition directly depends on the power density and duration of the laser treatment, which are registered by the phonon Raman spectra. After laser treatment, AFM measurements register additional small spherical islands on the surface. Analysis performed on irradiated and unirradiated samples showed significant changes in transmission spectra, X-ray diffraction (XRD) pattern, Verdet constant, magneto-optical property, and absorption coefficient. The material obtained after laser irradiation can be described as specific nanocomposite consisting of bismuth oxide and silicon oxide-based nano-objects (dimensions below 15 nm in diameter), which are arranged in a matrix of Bi₁₂SiO₂₀.

1. Introduction

Sillenite crystals belong to the Bi₁₂MO₂₀ group (where M = Si, Ge, and Ti) compounds, that have a body-centered cubic crystalline structure with the space group I23 [1]. Crystal Bi₁₂SiO₂₀ has parameters a = 1.01067 nm, Z = 2 (two identical motives in the unit cell). The density functional theory calculations presented bandgap energy of Bi₁SiO₂₀ as 3.43 eV [2]. Experimentally determined values are lower [3]. These optically active crystals can exhibit many strong effects such as magneto-optical, photo-induced, and electro-optical effects. Also, they possess numerous interesting properties, such as high values of piezo-electric, dielectric and elasto-optic constants, as well as high dark electric resistance [1]. These crystals, usually as bulk crystals, have widespread applications as active elements in many devices, such us optical limiting, holography, spatial light modulation, optical phase conjugation, optical memories fiber optic sensors, and Pockels cells [4–6].

Lasers have great applications in material processing [7] and their role is only getting more expanded. The surface of a single crystal can be lasering treated [8] whereby a thin surface layer of the material is transformed when it interacts with the laser beam. This process is strictly controlled with the laser beam wavelength and power, its duty cycle, and repetition rate. The final result of how material is modified depends on a sample, since all materials have unique properties that dictate how they will interact with the laser radiation [9, 10].

Raman spectroscopy is an established technique to measure local material properties [11]. As such, it is very suitable for research related to the surface of the sample. However, since it uses a laser for excitation, structural changes may occur on the surface of the sample caused by local heating. In some cases, these modifications can lead to the decomposition of the sample, which results in a changed Raman signal [12, 13]. Changes in the spectrum can be in the position and half-width of phonon lines on the spectrum of the starting material, as well as lead to the appearance of new lines caused by permanent modifications in the sample [14, 15].

In our previous paper [16], we registered the decomposition of Bi₁₂SiO₂₀ (BSO) single crystal due to femtosecond laser irradiation. By far-infrared spectroscopy and AFM measurements, the existence of bismuth oxide nano-objects on the surface of the sample was registered. XRD could not register these changes. Also, it was not possible to establish control parameters between the formed nano-objects and the conditions of the experiment because the sample was treated in advance. Also, for the same reason, it was not possible to determine the exact phase composition of nano-objects.

The aim of this work is to continue the investigation of the influence of locally induced heating, with an increase in the power density of the semiconductor laser during Raman measurements, on the Bi₁₂SiO₂₀ single crystal. In this way, direct results related to the current state of Bi₁₂SiO₂₀ decomposition will be provided, as well as parameters that can control that process. Complementary techniques such as X‐ray diffraction (XRD), atomic force microscopy (AFM), UV‐Vis transmission, and magneto‐optical measurements will be used in the characterization of the obtained materials.

2. Materials and Methods

The Czochralski technique was applied to grow Bi₁₂SiO₂₀ single crystal, which is described in more detail in Ref. [16]. In short, MSR 2 crystal puller controlled by a Eurotherm was used. A platinum crucible was used to contain the melt, which was placed in an alumina vessel on zircon–oxide wool. Crystal growth was occurred in an air. Bi₂O₃ and SiO₂ were used for the synthesis of crystals. Starting materials were mixed in 6 : 1 stoichiometric ratio. Optimal pull rate was chosen in the range 5-6 mm/h. Equations of the melt hydrodynamics were used to calculate the critical crystal diameter, d_c = 10 mm, and critical rotation, ω_c = 20 rpm. The crucible was not rotating during crystal growth. The crystal boule was cooled at ∼50°C/h down to a room temperature, after the crystal growth. Crystals grew in [111] direction, without core being observed. Finally, crystals were cut and polished.

Polished crystal samples were treated using Verdi G optical pumped semiconductor laser with a 532 nm wavelength with different irradiation times during Raman experiment.

Atomic Force Microscopy (AFM) was used to determine topography of the samples with NTEGRA prima from NT-MDT.

The X-ray diffraction (XRD) data was measured using an X-ray diffractometer (XRD) Rigaku Ultima IV, Japan. The PDXL2 v2.0.3.0 software, with reference to the diffraction patterns available in the International Center for Diffraction Data (ICDD) [17], was used for phase identification and data analysis.

The UV-Vis transmission spectra were collected in the 200–900 nm range using a Perkin-Elmer Lambda 4B UV-Vis spectrophotometer.

Raman spectra of prepared samples were obtained using backscattering configuration of Jobin Yvon T64000 spectrometer equipped with nitrogen cooled CCD detector. The spectra were recorded in the spectral range 80–650 cm⁻¹ at room temperature using a 532 nm Verdi G optical pumped semiconductor laser line.

Parameters such as Faraday rotation, bulk absorption, and optical activity were measured at 632.8 nm using a He-Ne laser. This was obtained by an orthogonal polarization detection polarimetric method [18].

3. Results

3.1. Raman Spectroscopy

Raman spectra of Bi₁₂SiO₂₀ (BSO) single crystal, nanocrystalline powders, and thin films have been measured and analyzed in the past [19–22]. Identification of the observed peaks was performed on the basic of the factor group analysis for the SiO₄ tetrahedra, OBi_3, and Bi₃O₄ structural fragments. The Raman spectrum of the our Bi₁₂SiO₂₀ single crystal is shown in Figure 1(a). The spectrum was recorded with a laser power density of 0.1 mW/μm² and the measurement time of 5 s, which did not cause structural changes in the sample. The spectrum of Bi₁₂SiO₂₀ exhibits intense modes at about 87, 97, 104, 128, 144, 167, 176, 204, 269, 322, and 536 cm⁻¹. As expected, our spectrum from Figure 1(a) is identical to the literature data [19–22].

(a)

(b)

(c)

Raman spectra of a Bi₁₂SiO₂₀ single crystal recorded consecutively at different laser powers (0.5–2 mW/μm²) and the recording time of each measurement of 30 s, at the same place on the sample are shown in Figure 1(b). The intensity of the peaks registered in Figure 1(a) increases with increasing laser power. In addition, starting with the laser power of 0.7 mW/μm² additional structures were seen on the spectra at about 122, 235, 456, and 487 cm⁻¹. They are significantly weaker than already registered phonons, but their intensity also increases with increasing laser power. The result was checked with the same laser power, but with a measurement times of 1 s and 60 s. Raman spectra of Bi₁₂SiO₂₀ single crystal recorded at laser power density of 1.5 mW/μm² and different recording times at different locations on the sample are shown in Figure 1(c). A very short 1 s measurement excites a spectrum similar to that in Figure 1(a). An increase in recording time leads to the same effect registered in Figure 1(b). To explain the registered effect, it was necessary to do additional experiments.

3.2. AFM

Figure 2 shows the results of AFM measurements of the Bi₁₂SiO₂₀ single crystal and the same sample after the Raman measurements (shown in Figure 1(c)). In Figure 2(a), we can clearly see that the surface of the untreated sample is quite smooth with no visible cracks, and only traces of mechanical polishing can be seen. Figures 2(b) and 2(c) show the surface of the sample after laser treatment of 1.5 mW/μm², according to the procedure described in Section 3.1, with two different time lengths of each measurement (30 s and 60 s), respectively. Nano-objects, small white dots in the images, with a diameter of about 11 nm (Figure 2(b)) and 15 nm (Figure 2(c)) were observed on both images. In Figure 2(c) we see that the density of nano-objects is significantly higher than that registered in Figure 2(b).

(a)

(b)

(c)

3.3. XRD Measurements

The XRD patterns of prepared BSO single crystal and BSO laser treated (1.5 mW/μm², 60 s) are presented in Figure 3. From the XRD pattern of untreated BSO single crystal (the bottom spectrum) it is clearly seen that all peaks correspond to Bi₁₂SiO₂₀. Results show that only selenite (Bi₁₂SiO₂₀) phase is present, which corresponds to the JCPDF Card No. 37-0485. When compared to laser treated BSO single crystal (upper spectrum), except silenite peaks are observed. These peaks correspond to: Bi₄O₇ (JCPDF Card No. 01-074-2352), Bi₂O₃ (00-057-0400, 00-051-1161, and 01-079-6679), and SiO₂ (01-071-5334) phases. All additional phases are marked with different symbols in Figure 3.

XRD results clearly and unequivocally show the influence of locally induced heating with laser power on Bi₁₂SiO₂₀ single crystal as the separation of new phases in the form of different Bi₄O₇, Bi₂O₃, and SiO₂. These results explain the appearance of additional structures seen on the Raman spectra whose intensity increases with increasing laser power and measurement time. The appearances of secondary phases also explain the phenomenon of additional small white dots (nano-objects) in the AFM images of laser-treated samples.

3.4. UV-Vis Spectroscopy

In Figure 4(a) the results of transmission measurements of BSO samples in the UV-VIS region are presented. It is noticeable that for the laser-treated sample in the area of wavelength above 550 nm, the transmittance was reduced by about 5%. To determine the value of the energy gap eg, we using the well-known Kubelka–Munk theory (see for example, [3] and the literature cited there). The results of the analysis are shown in Figures 4(b) and 4(c).

(a)

(b)

(c)

For the untreated BSO single crystal, an energy gap value of 2.57 eV was obtained. This energy is lower than accepted band gap energy of BSO [3]. This smaller energy was associated with defect centers, as analyzed in [23–25]. A value of 2.47 eV was obtained for the laser-treated sample. Such a simple model cannot provide a complete picture of the modifications made in the sample, but it can indicate a macroscopic change, i.e. a parameter that is in some way its consequence.

3.5. Optical Activity, Faraday Rotation, and Bulk Absorption

Optical activity and Faraday rotation were measured by the free space setup described in [26]. It was noted that significant light scattering in the sample causes cross-talk of the two channels for the orthogonal polarizations detection. Therefore, birefringent crystal was replaced with a Wollaston prism decoupling the channels but also spoiling evenness of channels losses and forcing the use of two photodiodes. Two channels gain that include optoelectronic conversion efficiencies were equalized by transimpedance resistors.

Background light influence was eliminated using an optical chopper and lock-in amplifier. Laser’s polarization instability was converted to light irradiation fluctuations by polarizing prism mounted after the laser. Δ/Σ normalization method used is insensitive to light irradiation fluctuations but introduces another problem. It was also noted that treated BSO induces more depolarization of light compared to untreated one. This is partially the consequence of nano-objects at the surface of the treated BSO. Contribution of depolarized light is canceled in the subtraction but not in the sum leading to reduced result for Optical activity and Faraday rotation. It is possible to compensate this effect but only for particular crystal orientation. Instead of that we averaged the results for tree different crystal orientations. Results are presented in Table 1 having in mind scattering while measuring the absorption coefficient lens was used after crystal to focus the light on photodiode. Verdet constant was divided by absorption coefficient to obtain the magneto-optical quality of sample.

4. Discussion

As far as we know, [18] preparation technique which was used ensured maximum quality samples in the limits corresponding to the starting components purity. In the case of Bi₁₂GeO₂₀ [27], the positive effect of laser radiation on optical characteristics was registered only in materials obtained from starting materials of lower quality. With quality single crystals, it was not possible to improve the optical parameters in this way. This is also the case with Bi₁₂SiO₂₀, which we treated with a laser, i.e. we have a change of several percentages at maximum laser power.

We can interpret the additional structures from Figures 1(b) and 1(c) as follows. Figure 2 clearly shows nano-objects with dimensions of about 15 nm with very narrow dimensional distributions. It is easy to connect these nano-objects with the new phases from Figure 3, registered for the treated sample. These new phases show their characteristics on Raman spectra as well. First, four polymorphic phases of bismuth–oxide are known: the one stable at the room temperature, orthorhombic α-Bi₂O₃, and three high–temperature ones: β-, δ-, and γ-Bi₂O₃ [28–30]. Since new structures are visible even at relatively low laser powers, as well as on XRD at room temperature, we can conclude that only the orthorhombic α-Bi₂O₃ phase is present. In this way, we easily connect the additional structures in the Raman spectra at around 122 cm⁻¹ and 456 cm⁻¹ with this phase [31]. XRD also registered the Bi₄O₇ phase. This phase has a phonon at 118 cm⁻¹ [32], so the presence of the influence of this phase on the phonon registered at 122 cm⁻¹ in our experiment is not excluded. The situation is much clearer for the phonon at 486 cm⁻¹. This phonon is associated with Bi-O stretching vibrations in distorted linked BiO₆ units in the previously registered Bi₄O₇ phase [33, 34].

On the other hand, the diversity of SiO₂-based phases is even greater [35]. However, we think that in our case, SiO₂ clusters have T_d symmetry and corresponding Raman modes at 235 cm⁻¹. Also, experimentally at 463.6 cm⁻¹ and theoretically at 461 cm⁻¹, there is a SiO₂ phonon of the same symmetry. Therefore, the origin of the phonon at 456 cm⁻¹ cannot be accurately determined, i.e. due to the weak intensity of the experimental result, it is difficult to separate the influence of this phonon from that of α-Bi₂O₃. This result is in agreement with Ref. [19, 20].

In this way, it is clearly shown that laser heating during the Raman experiment produces nano-objects consisting of bismuth oxide and silicon oxide arranged in a matrix of Bi₁₂SiO₂₀ single crystal. This structure by its composition can be classified as a nanocomposite because the dispersed phase is in the nanometric size, with the specificity that the nano-object is formed from the same material, or its parts, such as a matrix.

Our results presented in this paper can be interpreted in at least two ways. First, it can be said that the made modification did not lead to the improvement of the characteristics of the observed material. That is true in principle. But this is practically expected, because the starting material, BSO single crystal, was obtained from ultrapure components, which led to the exceptional optical quality of the sample, as it was the case with the Bi₁₂GeO₂₀ crystal [18, 27].

However, the modification made led to a partial, but almost controlled, decomposition of the base material. A stable structure was created, which gives the prospect of using nano-objects in robust electronics. Namely, due to their extremely small sizes, nanomaterials (one, two, or three dimensions of less than 100 nm) cannot be used in large scale, particularly as long-bearing materials in engineering applications. For this it has long been a desire to develop bulk composites incorporating these nanomaterials (for example, nanocomposites) to harness their extraordinary properties in bulk applicable materials. Initial ideas and principles are given in [36]. The most important fact is that the characteristics of the nanomaterials are fundamentally different in comparison with the bulk materials [37]. In our opinion, this way of obtaining specific nanocomposites deserves attention.

In addition, in this paper, it is once again shown, this time directly, that during Raman measurement of complex structures and materials, the used laser power should be taken into account. It is very useful to measure Raman spectra with high laser powers. The spectrum is more intense, and the lines are more pronounced. The same applies to the duration of the measurement. However, in those cases, partial decomposition of the observed material or structure may occur, which results in the existence of lines on the spectrum do not belong to the original material, but they are the result of local and partial decomposition. Such results lead to wrong conclusions.

5. Conclusion

High-quality single crystal Bi₁₂SiO₂₀, with parameters of 2.57 eV, Verdet constant of 61 rad/Tm, and magneto-optical quality of 0.59 rad/T growth by the Czochralski technique. We used 532 nm line of Verdi G optical pumped semiconductor laser, during the Raman experiment, to modify the surface on a Bi₁₂SiO₂₀ single crystal. By measuring phonon spectra with Raman spectroscopy, starting from the laser power density of 0.7 mW/μm², and irradiation time greater than 1 s, we have registered new structures at about 122, 235, 456, and 478 cm⁻¹. AFM measurements confirm that the Bi₁₂SiO₂₀ crystal has decomposed on the surface, and newly formed bismuth oxide and silicon oxide-based nano-objects in the Bi₁₂SiO₂₀ matrix was found. This decomposition of Bi₁₂SiO₂₀ single crystal led to small changes in the electrical and magneto-optical characteristics of the base material. This structure by its composition can be classified as a nanocomposite because the dispersed phase is in the nanometric size, with the specificity that the nano-objects are formed from the same material or its parts, such as a matrix.

Data Availability

Data are available upon reasonable request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

This research was supported by the Science Fund of the Republic of Serbia, Grant no. 7504386, Nano object in own matrix–Self composite–NOOM-SeC.

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Copyright © 2023 Nebojsa Romcevic et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Journal of Spectroscopy

Effect of Laser Heating on Partial Decomposition of Bi12SiO20 (BSO) Single Crystal: Raman Study

Abstract

1. Introduction

2. Materials and Methods

3. Results

3.1. Raman Spectroscopy

3.2. AFM

3.3. XRD Measurements

3.4. UV-Vis Spectroscopy

3.5. Optical Activity, Faraday Rotation, and Bulk Absorption

4. Discussion

5. Conclusion

Data Availability

Conflicts of Interest

Acknowledgments

References

Copyright

Effect of Laser Heating on Partial Decomposition of Bi₁₂SiO₂₀ (BSO) Single Crystal: Raman Study