# Spectroscopic Properties of Sm 3+ Doped Lithium Zinc Borosilicate Glasses

N Jaidass, C Krishna Moorthi, M Mohan Babu, M Reddi Babu

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N Jaidass, C Krishna Moorthi, M Mohan Babu, M Reddi Babu. Spectroscopic Properties of Sm 3+ Doped Lithium Zinc Borosilicate Glasses. Mechanics, Materials Science & Engineering Journal, 2017, 10.2412/mmse.4.50.890. hal-01502475

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Distributed under a Creative Commons Attribution 4.0 International License
# Spectroscopic Properties of Sm³⁺Doped Lithium Zinc Borosilicate Glasses

N. Jaidass¹,², C. Krishna Moorthi¹, A. Mohan Babu¹,², M. Reddi Babu¹,²

1. School of Advanced Sciences, VIT University, Vellore - 632 014, India

2. Dept. of Physics, Chadalawada Ramanamma Engineering College, Tirupati - 517 506, India

<figure><img src="image_2.png" /></figure>

DOI 10.2412/mmse.4.50.890 provided by [Seo4U.link](https://seo4U.link)

**Keywords:** LZBS Glasses, Quenching technique, Photonic devices, Optical amplifiers.

**ABSTRACT.** For spectroscopic analysis, the Sm³⁺ ions doped with lithium zinc borosilicate (LZBS) glasses were prepared by the conventional melt quenching technique. The prepared glasses were characterized by the XRD, SEM, optical absorption, luminescence and decay measurements. The XRD spectrum clearly revealed that the LZBS glass is amorphous in nature and the SEM spectrum conformed the same. The UV-VIS-NIR absorption spectra revealed seventeen peaks at 360, 374, 389, 402, 416, 437, 462, 476, 526, 562, 943, 1076, 1224, 1369, 1471, 1521 and 1584 nm corresponding to the ⁶H₅/₂→⁴D₃/₂, ⁶P₇/₂, ⁴L₁₅/₂, ⁶P₃/₂, ⁶P₅/₂, ⁴G₉/₂, ⁴I₁₃/₂, ⁴I₁₁/₂, ⁴F₃/₂, ⁴G₅/₂, ⁶F₁₁/₂, ⁶F₉/₂, ⁶F₇/₂, ⁶F₅/₂, ⁶F₃/₂, ⁶H₁₅/₂ and ⁶F₁/₂ transitions, respectively. The Judd-Ofelt intensity parameters (Ω₄, Ω₄ and Ω₆) have been determined from the absorption data and these parameters are found to follow the trend as Ω₄>Ω₆>Ω₆. Photoluminescence spectra recorded by the excitation wavelength of 402 nm, revealed four emission peaks at 562, 598, 645 and 713 nm corresponding to ⁴G ₅/₂→⁶H₅/₂, ⁶H₇/₂, ⁶H₉/₂ and ⁶H₁₁/₂ transitions, respectively. Radiative transition probabilities (A_R) peak stimulated emission cross-sections (σ_e), experimental (β_exp) and calculated (β_R) branching ratios were determined for different emission transitions. The nature of decay curves of ⁴G₅/₂ level for different Sm³⁺ ions concentrations in the LZBS Smx glasses has been analyzed using Inokuti-Hirayama (I-M) model and the lifetimes (τ_exp) are found to decrease with increase of Sm³⁺ ions concentrations.

**Introduction.** Rare earth doped glasses are more useful materials, in the development of fiber amplifiers, sensors, high optical data storage, laser media and quantum electronic devices [1-4]. For the design of optical devices, host glasses with low phonon energies are essential. Among rare earth ion doped glasses, borosilicate glasses are popular host materials due to their good transparency and easy to draw into fibers for different laser applications. Borosilicate glasses possess excellent optical properties like fluoride glasses with higher chemical durability and better mechanical properties [5-7]. Moreover, the Sm³⁺, Dy³⁺ and Tb³⁺ ions emit orange, blue and green light, while the Pr³⁺ ions emit different colors depending on the concentration of dopant ions as well as surrounding environment. In the present work, the emission characteristics of Sm³⁺ ions in LZBS glasses are determined from the absorption, luminescence and decay measurements. J-O intensity parameters Ωₓ (λ= 2, 4 and 6) are determined from the experimental oscillator strengths. The radiative transition probabilities (A_R), experimental branching ratio (β_R), stimulated emission cross-section (σ_e), gain bandwidth (σ_e×Δλ_p) and optical gain (σ_e×τ_R) are evaluated. The concentration quenching phenomenon with concentration variation of Sm³⁺ ions and the mechanism involved has been discussed.

**Experimental.** LZBS glasses with chemical compositions of (30-x) H₃BO₃: 25SiO₂: 10Al₂O₃: 30LiF: 5ZnO: xSm₂O₃ were prepared with different Sm₂O₃ concentrations of 0.1, 0.5, 1.0 and 2.0 mol % by the conventional melt quench technique and are labeled as LZBS Sm01, LZBS Sm05, LZBS Sm10, and LZBS Sm20. About 10g of the batch chemicals were thoroughly mixed and grinded to get homogeneous mixture and heated at 1200°C in an electric furnace for 3 hours and then the melt was poured onto a pre-heated brass plate. After casting, the glasses were annealed at 350°C for 7 hours to
remove thermal strains and stress. To determine the amorphous nature of the host glass, the XRD spectrum was recorded using the Philips X'Pert - MPD X-ray diffractometer using Cu Kα radiation. The optical absorption spectra were recorded in the region 200 - 2200 nm using JASCO V-770 UV-VIS-NIR spectrophotometer and the photoluminescence excitation and decay measurements were recorded using the FLS-980 spectrofluorimeter.

**Results and discussion.** The XRD spectrum of undoped LZBS glass is shown in the Fig. 1. It revealed the absence of sharp peaks in the host LZBS glass and SEM image is shown in the Fig. 2 conformed the amorphous nature of LZBS glass.

<figure><img src="image_3.png" /><figcaption>Fig. 1. (a) XRD pattern of LZBS Sm0.0 glass. Fig. 1. (b) SEM image of LZBS Sm0.0 glass.</figcaption></figure>

**Optical analysis.** To study the optical absorption properties of LZBSSm10 glass, the absorption spectra were recorded in the UV-VIS and NIR regions are shown Figs. 2(a) & (b). The intensities of absorption bands are determined by their oscillation strengths (f), which are directly proportional to the area under the absorption bands. The assignment of absorption bands are made by comparing the band positions with those reported by Carnall et al. [8].

<figure><img src="image_4.png" /><figcaption>Fig. 2. Optical absorption spectrum of LZBSSm10 glass in the (a) UV-VIS regions (b) NIR region.</figcaption></figure>

The observed $^6H_{5/2} \rightarrow ^6P_{3/2}$ hypersensitivity transition at 402 nm exhibited highest intensity compared to other transitions. The Judd-Ofelt theory [9, 10] has been adopted for the analysis of oscillator
strengths of the absorption bands in order to know the nature of bonding between the rare earth ions and the surrounding ligands as well as the symmetry around rare earth ions. The experimental ($f_{exp}$) and calculated ($f_{cal}$) oscillator strength are determined by finding the relative areas of absorption bands and also using the equations given in previous reports by Reddi Babu et al. [11]. The evaluated J-O intensity parameters of LZBSSm10 glass are compared with those of other Sm³⁺ doped glasses [12-19] in the Table 1. All the J-O parameters follow the trend as $\Omega_2 > \Omega_4 > \Omega_6$. In the present investigation, the considerably higher magnitude of $\Omega_2$ indicates lower degree of symmetry around the Sm³⁺ ion and relatively weaker covalence of active ion-oxygen bond.

<table><caption>Table 1. Comparison of Judd-Ofelt intensity parameters (in $10^{-20}$ cm²) of Sm³⁺ ions in LZBSSm10 glass along with other reported glasses.</caption><thead><tr><th>System</th><th>Ω<sub>2</sub></th><th>Ω<sub>4</sub></th><th>Ω<sub>6</sub></th><th>Trend</th><th>Reference</th></tr></thead><tbody><tr><td>LZBS Sm10</td><td>2.94</td><td>9.9</td><td>6.89</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>Present work</td></tr><tr><td>NSBaP</td><td>0.33</td><td>8.60</td><td>3.92</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[12]</td></tr><tr><td>L5BS10</td><td>6.21</td><td>9.68</td><td>7.16</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[13]</td></tr><tr><td>Bismuth borate</td><td>2.10</td><td>5.54</td><td>4.58</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[14]</td></tr><tr><td>Fluorozincate</td><td>0.68</td><td>3.77</td><td>2.15</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[15]</td></tr><tr><td>Phosphate</td><td>1.50</td><td>3.75</td><td>1.89</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[16]</td></tr><tr><td>LBTAF</td><td>0.27</td><td>2.52</td><td>2.47</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[17]</td></tr><tr><td>LCZSFB</td><td>3.29</td><td>9.16</td><td>5.28</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[18]</td></tr><tr><td>ZNBS</td><td>0.30</td><td>3.82</td><td>3.65</td><td>Ω<sub>4</sub> &gt; Ω<sub>6</sub> &gt; Ω<sub>2</sub></td><td>[19]</td></tr></tbody></table>

**Photoluminescence and radiative analysis.** The emission spectra recorded in the range 500–800 nm for the LZBSSmx (x = 0.1, 0.5, 1.0 and 2.0 mol %) glasses are shown in the Fig. 3. These spectra revealed four emission bands at 562, 598, 645 and 767 nm from the excited ⁴G₅/₂ level to the ⁶H₅/₂, ⁶H₇/₂, ⁶H₉/₂ and ⁶H₁₁/₂ lower transition levels of Sm³⁺ ion. Among these emissions, the band located at 598 nm corresponding to ⁴G₅/₂→⁶H₇/₂ is the most intense one. In addition, the emission bands at 598, 647 and 709 nm are important because they are located at the longer wavelength region. The transitions ⁴G₅/₂→⁶H₅/₂ (562 nm) and ⁴G₅/₂→⁶H₇/₂ (592 nm) contain both electric and magnetic dipole contributions, obeying the selection rules, i.e $\Delta J = 0, \pm 1$, while the other two emission transitions ⁴G₅/₂→⁶H₉/₂ and ⁴G₅/₂→⁶H₁₁/₂ are purely electric dipole transitions [20, 21]. It is observed from the Fig. 3, that the emission intensities are increased upto 0.5 mol% of Sm³⁺ ions concentrations and then decreased at higher concentrations. The luminescence efficiency of Sm³⁺ ions doped LZBS emission transitions are found by evaluating the radiative parameters such as transition probabilities ($A_R$), branching ratios ($\beta_R$), radiative lifetimes ($\tau_R$) and peak stimulated emission cross sections ($\sigma_e$) for the $\Psi J \rightarrow \Psi' J'$ emission transitions by using the equations given in previous reports [11]. The efficiency of laser transition mainly depends on the stimulated emission cross-section ($\sigma_e$), gain bandwidth ($\sigma_e \times \Delta\lambda_{eff}$) and optical gain parameters ($\sigma_e \times \tau_{exp}$) [22, 23]. The laser characteristic parameters for the ⁴G₅/₂→⁶H₇/₂ and ⁴G₅/₂→⁶H₉/₂ transitions in the LZBSSm05 glass are compared with those of Sm³⁺ doped other hosts [24-29] in Table 2. It is observed that, the $\sigma_e$, $\beta_R$ and $\beta_{exp}$ values and are comparable with the reported values in different hosts.
<figure><img src="image_5.png" /><figcaption>Fig. 3. Photoluminescence spectra of Sm³⁺ ions in LZBSSmx (x = 0.1, 0.5, 1.0 and 2.0 mol %) glasses.</figcaption></figure>

<table><caption>Table 2. Comparison of radiative parameters such as emission band positions (λp,nm), effective band widths (Δλeff nm), radiative transition probabilities (AR S⁻¹), peak stimulated emission cross section (σe(×10⁻²² cm²)), calculated and experimental branching ratios (βR & βexp) LZBSSm05 glass with other glasses.</caption><thead><tr><th colspan="6">Transition <sup>4</sup>G<sub>5/2</sub>→<sup>6</sup>H<sub>7/2</sub></th><th colspan="6">Transition <sup>4</sup>G<sub>5/2</sub>→<sup>6</sup>H<sub>9/2</sub></th></tr><tr><th colspan="6">Parameters</th><th colspan="6">Parameters</th></tr><tr><th>System</th><th>λ<sub>p</sub></th><th>Δλ<sub>eff</sub></th><th>A<sub>R</sub></th><th>σ<sub>e</sub></th><th>β<sub>exp</sub></th><th>β<sub>cal</sub></th><th>λ<sub>p</sub></th><th>Δλ<sub>eff</sub></th><th>A<sub>R</sub></th><th>σ<sub>e</sub></th><th>β<sub>exp</sub></th><th>β<sub>cal</sub></th></tr></thead><tbody><tr><td>LZBSm05(Present)</td><td>598</td><td>12.90</td><td>253</td><td>12.99</td><td>0.48</td><td>0.43</td><td>645</td><td>15.02</td><td>182</td><td>10.8</td><td>0.35</td><td>0.31</td></tr><tr><td>SLBiBSm05 [24]</td><td>603</td><td>26.4</td><td>177.8</td><td>8.34</td><td>0.58</td><td>0.37</td><td>649</td><td>29.1</td><td>118</td><td>7.05</td><td>0.19</td><td>0.26</td></tr><tr><td>TWZSm10 [25]</td><td>602</td><td>16.73</td><td>346</td><td>7.7</td><td>0.53</td><td>0.46</td><td>649</td><td>17.19</td><td>255</td><td>7.4</td><td>0.25</td><td>0.29</td></tr><tr><td>PKAPN Sm10 [26]</td><td>598</td><td>11.2</td><td>227</td><td>11.5</td><td>0.57</td><td>0.47</td><td>645</td><td>11.7</td><td>158</td><td>10.4</td><td>0.25</td><td>0.33</td></tr><tr><td>0.5LBTPS [27]</td><td>605</td><td>9.3</td><td>215</td><td>13.14</td><td>0.55</td><td>0.43</td><td>649</td><td>9.5</td><td>140</td><td>11.0</td><td>0.20</td><td>0.28</td></tr><tr><td>PbFPSm10 [28]</td><td>601</td><td>13.96</td><td>185</td><td>8.98</td><td>0.57</td><td>0.43</td><td>648</td><td>17.04</td><td>171</td><td>9.18</td><td>0.22</td><td>0.40</td></tr><tr><td>TMZNB [29]</td><td>601</td><td>14.7</td><td>232</td><td>11.70</td><td>0.57</td><td>0.4</td><td>647</td><td>13.8</td><td>212</td><td>11.0</td><td>0.22</td><td>0.36</td></tr></tbody></table>

**Decay analysis.** Fig.4 shows the decay profiles of <sup>4</sup>G<sub>5/2</sub> excited level for different concentrations of Sm³⁺ ions in LZBSSmx (x=0.1, 0.5, 1.0 and 2.0 mol %) glasses obtained with excitation wavelength of 402 nm. The decay curves exhibited single exponential nature at lower concentrations (0.1 mol %) and turned into the non-exponential at higher concentrations (0.5, 1.0 and 2.0 mol %) of Sm³⁺ ions. The single exponential nature is due to either faster decay of excited Sm³⁺ ions or the negligible interaction between the Sm³⁺ ions at lower concentrations. The experimental lifetimes with the increase of Sm³⁺ ions concentration are found to be decreased as 2.23, 1.40, 0.82 and 0.41 ms corresponding to the LZBSSm01, LZBSSm05, LZBSSm10 and LZBSSm20 glasses, respectively. In the present work, at lower concentrations of Sm³⁺ ions (0.1 mol %), the decay curve is well fitted to
single exponential which indicates the absence of energy transfer between the Sm³⁺ ions, whereas at higher concentrations of Sm³⁺ (0.5, 1.0 and 2.0 mol%), the decay profiles turned into non-exponential due to non-radiative energy transfer of the excited ions. The calculated lifetime (τR) of the ⁴G₅/₂ level from the J-O theory for the LZBSSm05 is 1.68 ms.

<figure><img src="image_6.png" /><figcaption>Fig. 4. The decay profiles for the ⁴G₅/₂ excited level of Sm³⁺ ions in LZBSSmx glasses.</figcaption></figure>

**Summary.** Sm³⁺ ions doped lithium zinc borosilicate glasses (LZBS) were prepared by conventional melt quenching method, and are characterized by different analytical and spectroscopic measurements. The amorphous nature of glass has been confirmed by XRD profiles. The evaluated Judd-Ofelt intensity parameters (Ω₂, Ω₄ and Ω₆) were found to be in the order Ω₄ > Ω₆ > Ω₂ for all the LZBS Sm10 glass. From the emission spectra, it is observed that the intensities of emission peaks increased upto 0.5 mol% and decreased for 1.0 and 2.0 mol% of Sm³⁺ ions concentrations. The radiative parameters such as transition probabilities (Aₑ), total transition probabilities (Aₜ), branching ratios (βₑ), radiative lifetimes (τₑ) and peak stimulated emission cross sections (σₑ) were calculated for the emission transitions. The large stimulated emission cross sections observed for the ⁴G₅/₂→⁶H₇/₂ and ⁴G₅/₂→⁶H₉/₂ transitions suggests that, the present glasses are excellent hosts for laser active materials. The decay profiles of the ⁴G₅/₂ excited level exhibited single exponential at lower concentrations of Sm³⁺ ion and turned into non-exponential nature at higher concentrations.

**Acknowledgement.** One of the authors Dr.A.Mohan Babu would like to thank DST-SERB, New Delhi for the sanction of research project Lr. No. SR/FTP/PS-109/2012 and DAE - BRNS Mumbai for the sanction of major research project No.2012/34/72. Also, N.Jaidass is thankful to DST-SERB, New Delhi for the financial support in the form of Project Assistant in the above project.

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Cite the paper
N. Jaidass, C. Krishna Moorthi, A. Mohan Babu, M. Reddi Babu, (2017). *Spectroscopic Properties of Sm3+Doped Lithium Zinc Borosilicate Glasses*. Mechanics, Materials Science & Engineering, Vol 9. DOI: 10.2412/mmse.4.50.890