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Vol. 9. Issue 1.
Pages 59-66 (January - February 2020)
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Vol. 9. Issue 1.
Pages 59-66 (January - February 2020)
Original Article
DOI: 10.1016/j.jmrt.2019.10.029
Open Access
The influence of Ba2+ and Sr2+ ions with the Dy3+ ions on the optical properties of lead borate glasses: experimental and Judd–Ofelt comparative study
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Aly Okashaa,
Corresponding author
aliokasha2@yahoo.com

Corresponding author.
, A.M. Abdelghanya,b, S.Y. Marzoukc
a Spectroscopy Department, Physics Division, National Research Center, 33 ElBehouth St., Dokki, 12311, Giza, Egypt
b Basic Science Department, Horus University, International Coastal Rd, New Damietta, Kafr Saad, Damietta, Egypt
c Basic and Applied Science, Faculty of Engineering, Arab Academy of Science and Technology, Al-Horria, Heliopolis, Cairo, Egypt
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Tables (6)
Table 1. Glass symbols, direct and indirect optical band gap, Eg; glass density, D; and the refractive index n.
Table 2. FTIR band position and assignments.
Table 3. Calculated (fcal) and (fexp) experimental oscillator strengths along (from the ground state, 6H15/2), with J–O parameters of the prepared glass samples.
Table 4. Comparison of Judd–Ofelt parameters (×10−20cm2) in Dy3+ glasses.
Table 5. Calculated refractive indexes for prepared glass samples.
Table 6. Calculated branching ratio (β) and lifetime (τ, ms) for prepared glass samples.
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Abstract

Two glasses compositions (50B2O3–30PbO–20SrO–xDy) and (50B2O3–30PbO–20BaO–xDy) where x=0.0.5%, and 1.0% in wt.% ratio were prepared using melt quenching technique in order to investigate the effect of Ba2+ and Sr2+ ions in Dy3+ ions doped lead borate glass. The optical properties such as bandgap and the refractive index distribution were examined using UV–vis-NIR absorption spectroscopy. The FTIR absorption spectra of all prepared samples were similar except for the metallic bands in the fingerprint region. The obtained experimental data were compared with theoretical data calculated by Judd–Ofelt framework. The Judd–Ofelt parameters Ωλ (λ=2, 4 and 6) were calculated and the trend was Ω2<4<6 which is the common trend. The experimental oscillator strength  (fexp), the calculated oscillator strength  (fcal), the estimated refractive indexes (n) at each transition, the lifetime of radiative transitions (τ), the branching ratio (β), the absorption cross-section (σabs(λ)) and the emission cross-section (σemis(λ)) were also estimated and discussed. The optical gain coefficient (G(λ)) was calculated not only for the most intense emission transition but also other emission peaks. The obtained results indicated that the prepared samples are promising materials for laser emission and optical communication applications.

Keywords:
Lead borate glasses
Optical properties
Judd–Ofelt theory
Full Text
1Introduction

During the last two decades, the using of the glasses material attracts enormous attention. Among the glasses material the borate glass containing transition metals, such as ZnO, PbO, TeO2 Bi2O3, MgO, CaO, SrO, and BaO, attracts great attention due to the ability to tailoring its properties to fit special applications. Recent developments in the field of borate glasses have led to a renewed interest in the fields of leasing and Opto-communications materials, optical filters and photonic devices [1]. Several attempts have been made to investigate the modified lead borate glasses materials. In that manner, Shaw et al. [2] and Zuh et al. [3] studied the phase separation of the lead borate glasses. Besides, Xi et al. [4] and Wang et al. [5], were reported that the ratio of PbO/B2O3 is playing an essential role in the structure of the glass network. Adding heavy metal oxides, such as BaO and SrO, to the lead borate glasses is one of the most widely used methods to tailoring the optical properties and radiation shielding of the glasses [6]. The great change in the optical properties of the glasses was experienced by adding a rare earth element to the structure of the glasses. Pisarska et al. [7] studied the lead borate glass contains Dy3+ ions and investigates the luminance properties in the presence of Al2O3 and WoO3. In their study, the absorption and luminance properties of the glass were investigated and compared by the estimated theoretical values using Judd–Ofelt (J–O) calculation. The same group studied the Dy3+ luminance transitions 6H11/2 at 662nm, 6H113/2 at 573nm and 6H15/2 at 480nm [8]. In addition, the yellow/blue luminescence of trivalent Dy was studied as a function of the B2O3/PbO ratios in the presence of Cr3+ as an alkaline metal [9]. So far, however, The research to date has tended to focus on investigation the luminance properties of lead borate glasses containing Dy3+ in the visible spectral region rather than the IR spectral region [7–9].

In the present study two glass series were prepared, (50B2O3–30PbO–20BaO–XDy), and (50B2O3–30PbO–20SrO–xDy) where x=0, 0.5% and 1%. The study has tended to focus on studying the optical properties of the lead borate glass containing Dy3+ ions in the presence of two alkali earth metal oxides (BaO and SrO) in both the visible and the IR region. The experimental data will compare with the theoretical data obtained from the J–O framework to estimate the absorption and luminance characteristics to investigate the suitability of the studied glasses in the optical communication fiber.

2Experimental details2.1Samples preparation

Two glass systems of nominal composition (50B2O3–30PbO–20SrO–xDy) and (50B2O3–30PbO–20BaO–xDy) where x=0.0.5%, and 1.0% in wt.% ratio, were prepared using pure chemical reagents including orthoboric Boric acid, H3BO3 (Laboratory Rasayan Sd Fine-Chem. Limited), lead Oxide, PbO (Sisco research Lab. India), Barium Oxide BaO, and Strontium Oxide, SrO from (Panreac Quimica SA, Espana), Dy3O2 (99.99%, Aldrich Chemical Co) which were used as received without any farther purifications. The melt quenching technique was used in glass synthesis under atmospheric conditions. In the typical method, weighted materials were mixed carefully and melted at 1100°C using an electric furnace for about 2h in platinum crucibles. In the next step, samples were cast in a stainless steel mold and transferred into a muffle furnace and kept at 400◦C for annealing for 2h, then the furnace was left to cool down to the room temperature overnight. Six samples were cut, polished and smoothed in 1cm×2cm (±0.1mm) rectangular shape with 2mm (±0.1mm) thickness. Finally, the samples named (base Ba), (0.5 Dy Ba), (1.0 Dy Ba), (Base Sr), (0.5 Dy Sr) and (1.0 Dy Sr) as shown in Table 1.

Table 1.

Glass symbols, direct and indirect optical band gap, Eg; glass density, D; and the refractive index n.

Sample symbol  Density, D (g/cm3) ±0.018  Direct optical band gap, ± 0.05 (eVIndirect optical band gap,± 0.05 (eVn 
Base Ba  4.87  2.91  3.42  1.43 
0.5 Dy Ba  4.80  2.91  3.41  1.43 
1.0 Dy Ba  4.76  2.91  3.43  1.43 
Base Sr  4.78  2.91  3.51  1.43 
0.5 Dy Sr  4.73  3.00  3.53  1.42 
1.0 Dy Sr  4.63  3.79  3.41  1.37 
2.2Glass density measurements

The traditional Archimedes method was used to determine the glass densities at room temperature by weighing the samples in both air (wtair) and weighed in submerged xylene (wtimmeresed). The density of the glass (D) is estimated from the equation:

where, 0.863 represents the xylene density in units of g/cm3. All measurements were performed in triplicate different samples for error elimination and estimation. The results of the density measurements were illustrated in Table 1.

2.3Optical absorption and infrared measurements

The absorption spectra of the samples under investigation were carried out using (JASCO model V730 Japan) spectrophotometer and the results were illustrate in Fig. 1. While, the FTIR spectra of the samples measured using (Bruker Model Vertex 70) Spectrometer using the KBr disc technique in the spectral range 4000–400cm−1. The FTIR spectra were demonstrated in Fig. 4.

Fig. 1.

UV–vis-NIR absorption spectra.

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3Results and discussion3.1Optical absorption

The absorption spectra in the UV–vis-IR spectral range from 300nm to 2000nm were illustrated in Fig. 1 the inset shows the sample (1.0 Dy Sr) focused on the range from 425nm to 550nm headed for identifying the two absorption peaks at 448nm and 476nm which corresponding to the transitions 4I15/2, 4F15/2 respectively. In addition, the mean figure showed other means six peaks at 748nm, 798nm, 900nm, 1090nm, 1267nm and 1672nm which are corresponding to the transitions, 6F3/2, 6F5/2, 6F7/2, 6F9/2, 6F11/2, and 6H11/2 respectively. The intensities of all transitions increase by increasing both Ba3+ and Sr3+ in the samples. The same results were reported by Marimuthu et al. [10]. They observed that the transitions 4I15/2, 4F15/2 of the Dy3+ ions are relativity weak comparing with the other transitions due to the strong host lattice absorption in the UV region.

3.2Calculations of the optical band gap

The fundamental optical band gap (Eopt) of the two studied glasses systems has no sharp edges as shown in Fig. 1. However, by using Beer–Lambert–Bouguer law, with simple modification the optical band gap energy calculated thought the equation [11]:

where m take values of ½ or 2 for direct allowed, indirect allowed transitions respectively, C is a constant and α is the absorption coefficient. The optical band gap values were obtained by extrapolating the linear region of the plot of Eq. (2) for m= ½ was illustrated in Fig. 2-a, while the fitted one for m=2 was illustrated in Fig. 2-b. It is observed that the value of the optical band gap in case of direct allowed or indirect allowed transitions for the Ba system glass nearly does not change with increase the Ba, and the value is around 2.97 and 3.41eV respectively. On the other hand, for Sr system, the direct-allowed decrease from 3.11 to 2.88eV, and indirect allowed transitions band gaps decreases from 3.50 to 3.41 by increasing the Sr content. However, directly allowed or indirect allowed band gap increase by increasing the Dy3+ in the samples. These results are in agreement with Marimuthu et al. [10] findings.

Fig. 2.

(a) Direct band gap for allowed transitions, (b) indirect band gab for allowed transitions.

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The optical band gap energies have been used to determine the different values of refractive index (n) by using Dimitrov and Sakka relation [12].

where Eg is the direct optical band gap for allowed transitions. The refractive index values enlisted in Table 1.

The reflectance distribution and the refractive index distribution are shown in Fig. 3-a and -b). The two figures indicate the sensitivity of the reflectance distribution and the refractive index distribution to the different transitions of Dy3+.

Fig. 3.

(a) Reflectance distribution and (b) represent the refractive index distribution.

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3.3FTIR absorption spectral data

FTIR absorption spectra are demonstrated in Fig. 4. The network observed in the studied two glasses systems are in the main three infrared bands. The band around ∼794cm−1 which related to the combination of both phosphate and borate groups (BO3 and BO4) with the first phosphate partner. The band <750–1150cm−1 related vibrations of both non-bridging PO2 groups and the stretching vibrations of BO3 groups. The band <1150–1600cm−1 related to (OH), POH, and BOH vibrations. In addition to the vibrations of metallic cations at about 460cm−1. The peak at about 2920 related to the hydrogen bonding, while the peak at about 3400 related to the OH group. There was no change in the absorption band between the studied samples. The previous study has reported the same results using NF3 phosphate glasses [13].

Fig. 4.

FTIR absorption spectra for all glass samples.

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The detailed band assignment are showed in the Table 2.

Table 2.

FTIR band position and assignments.

IR peak position (cm−1Peak assignment 
∼460  Vibrations of metal cations Ba2+ or Sr2+ 
∼617  Binding O—B—O 
∼694  Combination vibration of BO4 and PbO4 groups 
∼944  B—O—B linkage 
∼1214  Asymmetric stretching of B—O bonds from orthoborate groups 
∼1340  Presence of pyriborate, orthoborate groups containing BO3 
∼2923  Hydrogen bonding 
∼3430  OH group 
3.4Judd–Ofelt calculations

The calculations of the radioactive transitions properties illustrated by Judd–Ofelt theory [14,15] is important to understand the optical properties of the Dy3+ doped glasses in both the two matrix which contain Ba or Sr. The calculation in this work suggest that the calculated oscillator strength of an electronic dipole absorption transition, fcalS,LJ;S',L'J', from an initial state, S,LJ, to final excited state, S',L'J',  is depending on the Judd–Ofelt parameters Ωλ (λ=2,4,6) and is given by:

where m is the electron mass, h is the Plank’s constant, λ is the wavelength, n is the refractive index of the glass, and Uλ  is the doubly reduced matrix of the unit tensor obtained from Weber [16] were applied respectively. By applying the samples parameters (e, l, N, and OD(λ)) the experimental oscillator strength of an electronic dipole absorption transition fexp is given by:

where e is the electron charge, N is the number of active ions per unit volume, l is the sample thickness, and OD(λ) is the optical density. The Judd–Ofelt parameters Ωλ (λ=2,4,6) calculated using the least squares fitting method (r.m.s.)  according to the selection role │ΔS│=0, │ΔL│≤ 2, │ΔJ│≤ 2 [17].

The fitting accuracy between the calculated and the experimental parameters was estimated using the equation:

where P is the number of observed transitions on the absorption spectrum. However, the values of r.m.s. is small and the values of fcal and  fexp, is closed to each other. The results of the fcal, fexp, λ and r.m.s. are illustrated in Table 3.

Table 3.

Calculated (fcal) and (fexp) experimental oscillator strengths along (from the ground state, 6H15/2), with J–O parameters of the prepared glass samples.

Transition 6H15/2→  Wavele-ngth (nm)  Energy (cm-10.5 Dy Ba1.0 Dy Ba0.5 Dy Sr1.0 Dy Sr
      fexp  fcal  fexp  fcal  fexp  fcal  fexp  fcal 
6H11/2  1714.4  5833  2.9495  3.1383  1.7396  1.9244  2.240  2.498  2.7017  2.9463 
6F11/2  1294  7728  10.429  10.409  7.6416  7.6234  10.26  10.24  11.5734  11.549 
6H7/2  1097  9116  3.1675  0.1334  2.4002  0.083  3.427  0.113  3.6866  0.127 
6F7/2  907  11025  2.342  2.4199  1.745  1.8178  2.602  2.705  2.6537  2.7527 
6F5/2  804  12438  1.1763  1.1752  0.9019  0.7159  1.172  0.962  1.2913  1.0969 
6F3/2  756  22321  1.0826  0.2077  0.3164  0.1265  0.678  0.170  0.4528  0.1938 
Ω 2 10−20cm2      6.43315.48805.66368.4804
Ω 4 10−20cm2      4.09632.46945.24933.5443
Ω 6 10−20cm2      3.40482.07412.78613.1779
Ω4/ Ω6      1.2031.1901.8831.115
r.m.s.      0.86400.87470.86530.8321

Commonly, the parameter Ω2 is considered to be a metal covalency marker while the parameters Ω4 and Ω6 consider to be a host matrix rigidity marker. The values of the Ω2 of the sample (1.0 Dy Sr) in Table 3 indicate that the Dy–O covalency is strong and the asymmetry is low compared with the other samples. This result is in agreement with the results obtained by Refs. [18,19]. The value of Ω2 is increase by increasing the ratio of the Dy3+ in the two glasses matrices. The parameters Ω4 and Ω6 indicate that the sample (0.5 Dy Sr) is higher rigidity than the other samples and has also a higher spectroscopic quality factor (Ω4/Ω6). The factor (Ω4/Ω6) is a significant laser parameter in expecting the stimulated emission in a laser active media. The trend of the Ωλ is Ω2<4<6 which the common trend and also in agreement with the previous work [14]. Several attempts have been made to investigate the Judd–Ofelt parameters Ω2, Ω4, and Ω6 in addition to the factor (Ω4/Ω6). The present study has reported good fit values to the previous studies which reported in Table 4.

Table 4.

Comparison of Judd–Ofelt parameters (×10−20cm2) in Dy3+ glasses.

System  Reference  2  4  6  4/Ω6 
(30-x) (NaPO3)630PbO 40 B2O3+xDy2O3  [20]  6.37  0.34  2.16  0.199 
YAl3(BO3)4 (YAB)+Dy2O3  [21]  9.49  2.77  2.01  1.378 
(73_x)PbO–18B2O3–6Al2O3–3WO3–xDy2O3  [8]  4.90  0.94  2.07  0.454 
(79-x)B2O3+P2O5+10Li2O+10ZnO+1Dy2O3  [22]  2.95  1.20  1.79  0.670 
(99x)Li2CO3·xH3BO3·1Dy2O3  [23]  5.41  1.89  1.92  0.984 
(PbFPDy: P2O5+K2O+Al2O3+PbF2+Na2O+Dy2O3[24]  7.12  1.59  2.20  0.722 
30PbO–25Sb2O3–(45−x)B2O3–xDy2O3  [25]  5.81  1.13  2.68  1.116 
(50B2O3–30PbO–20SrO–xDy)  Present work  8.48  3.54  3.17  1.910 
(50B2O3–30PbO–20BaO–xDy)  Present work  5.48  2.46  2.07  1.115 

The calculated refractive indexes at every transition are demonstrated in Table 5. The data from this table can be compared with the data in Table 1 which shows a good fit.

Table 5.

Calculated refractive indexes for prepared glass samples.

Transition6H15/2→  Ba-Dy 0.5  Ba-Dy 1.0  Sr-Dy 0.5  Sr-Dy 1.0 
 
6H11/2  1.3589  1.4881  1.3798  1.5216 
6F11/2  1.4459  1.5740  1.4684  1.6013 
6H7/2  1.5074  1.6445  1.5296  1.6604 
6F7/2  1.2064  1.4173  1.2410  1.4425 
6F5/2  1.4028  1.5336  1.4303  1.5690 
6F3/2  1.4240  1.5513  1.4510  1.5860 

One of the most important advantages of the Judd–Ofelt analysis is the prediction of the radiative transition probabilities A(J,J') for the electric dipole transitions between excited states and the lower level of the Dy3+ which can be calculated using the parameters via the equation:

The lifetime of radiative an excited level is calculated by the inverse of the sum of A(J,J') values calculated overall terminal levels:

The luminescence branching ratio βJ,J' which, indicates the relative intensities of transitions from the excited, J, state to another level, J', is given by the relation:

The value of the branching ratio indicates the possibility of using the radiative transition band in the laser devices. Table 6 illustrates the values of the branching ratio of the most sensitive radiative transition and their corresponding radiate lifetime.

Table 6.

Calculated branching ratio (β) and lifetime (τ, ms) for prepared glass samples.

Transition6H15/2→  Ba-Dy 0.5Ba-Dy 1.0Sr-Dy 0.5Sr-Dy 1.0
  β  τ (ms)  β  τ (ms)  β  τ (ms)  β  τ (ms) 
6H11/2  0.9444  11.555  0.9094  13.798  0.9111  13.3924  0.9197  8.4993 
6F11/2  0.9537  1.2466  0.9492  1.2989  0.9487  1.2023  0.9477  0.8095 
6H7/2  0.4263  15.551  0.3911  17.352  0.3832  15.7759  0.3822  10.7177 
6F7/2  0.1627  0.3706  0.0671  0.1243  0.1215  0.2287  0.1275  0.1487 
6F5/2  0.6276  0.9518  0.4891  0.9250  0.4409  0.7708  0.5013  0.5754 
6F3/2  0.1749  0.7955  0.1358  0.7772  0.1374  0.7212  0.1511  0.5259 

It is apparent from this table that the two transition 6H11/2 and 6F11/2 in the demonstrated four samples is a quite possible candidate for using as gain media in 1700nm and 1300nm respectively (β≥0.5). the values of β in the rest of the transitions reveal that the not all the transition is high potential for using as gain media except for sample (0.5 Ba Dy) at the transition 6H7/2 and the samples (1.0 Ba Dy and 1.0 Sr Dy) at the transition 6F5/2. A Highly laser media candidate system was introduced by Vijayakumar et al. [22] using Dy3+ doped Zinc borophosphate glasses.

The absorption cross section at any transition σabs(λ) is given by the equation:

where N is the concentration of respective Dy3+ ions for each sample.

The corresponding emission cross section at the same transition (λ) is given by:

where Zl is the partition function for lower levels and Zu is the partition function for upper concerned in the measured optical transition, T is the room temperature and Ezl is the zero line energy for the transition between the lower Stark sublevels of the emitting and the receiving multiples. The values of (σemis) for the transition 6F11/2 (1267nm),which evaluated as hypersensitive transition (HST) in the IR region is about 2.0×10−20 for the sample (1.0 Dy Ba) and 2.9×10−20 for sample (1.0 Dy Sr).

Fig. 5 illustrates the predicted absorption and their corresponding emission for the transitions 6F7/2, 6F9/2, 6F11/2, and 6H11/2 in the four samples under investigation.

Fig. 5.

Predicted absorption and their corresponding emission for the transitions 6H11/2, 6F11/2, 6H7/2, and 6F7/2 (a) sample 0.5 Dy Ba, (b) sample 1.0 Dy Ba, (c) sample 0.5 Dy Sr, and (d) sample 1.0 Dy Sr.

(0.16MB).

The optical gain coefficient G(λ) is a very important function that helps to estimate the probability of operating laser wavelength using the equation [26,27]:

where P is the population inversion rate for laser transitions (4 transitions, N is the concentration of Dy3+ ions. The values of P were taken as 0, 0.1, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09 and 1.00. The distribution of the gain profiles for Dy3+ ions are illustrated in Fig. 6a–d.

Fig. 6.

Predicted gain coefficient Gλ for the prepared glasses doped with Dy3+ions (a) sample (0.5 Dy Ba), (b) sample (1.0 Dy Ba), (c) sample (0.5 Dy Sr), and (d) sample (1.0 Dy Sr).

(0.66MB).

Commonly the function G(λ) is calculated for the most intense emission peak, (at λ1267nm in our study), but what interesting in these study is calculating of the function G(λ) for the four transitions 6H11/2, 6F11/2, 6H7/2, and 6F7/2 which have the possibilities to use as operating laser wavelength media or in the optical communications fibers and laser emission wavelengths (β≥0.5).

4Conclusion

Successfully two glasses compositions (50B2O3–30PbO–20SrO–xDy) and (50B2O3–30PbO–20BaO–xDy) where x=0. 0.5%, and 1.0% in wt.% ratio, were prepared by melt quenching technique and from the experimental absorption spectra showed the regular transitions of the Dy3+ ions and the bandgap energy in both direct and indirect regimes remain without any significant change in case of the presence of Ba2+ while the band gap decreases then increases with the increase of Dy3+ in case of Sr2+ present. The mean regular transitions 6F3/2 (748nm), 6F5/2 (798nm), 6F7/2 (900nm), 6F9/2 (1090nm), 6F11/2 (1267nm), and 6H11/2 (1672nm) where observed in the absorption spectra. Also, the refractive index obtained from the experimental data agrees with the one obtained from theoretical calculations. The FTIR study confirmed there was no change in the absorption band between the studied samples. The existence of the structural units such as BO3, BO4 and PO4 and the presence of non-bridging oxygen with increasing Dy3+ ions concentration were identified. The Judd Ofelt calculations reveal that the sample (1.0 Dy Sr) has a strong Dy-O covalency and low asymmetry comparing with the other samples. On the other hand, the parameters Ω4 and Ω6 indicate that the sample (0.5 Dy Sr) is higher rigidity than the other samples and has also a higher spectroscopic quality factor (Ω4/Ω6). The obtained results were in good fit with the previous work. In addition, the results of this study showed that the two transition 6F11/2 and 6H11/2 in the demonstrated the four samples is a quite possible candidate for using as gain media in ≈1267nm and 1672nm respectively (β≥0.5) in the IR region. On the other hand, the function G(λ) for the four transitions 6H11/2, 6F11/2, 6H7/2, and 6F7/2 in the visible region have the possibilities to use as operating laser wavelength media or in the optical communications fibers and laser emission wavelengths.

Conflicts of interest

The authors declare no conflicts of interest.

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Journal of Materials Research and Technology

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