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Optics Express

Optics Express

  • Editor: C. Martijn de Sterke
  • Vol. 19, Iss. 27 — Dec. 19, 2011
  • pp: 26529–26535
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Broadband near-infrared emission in Tm3+-Dy3+ codoped amorphous chalcohalide films fabricated by pulsed laser deposition

Senlin Yang, Xuefeng Wang, Haitao Guo, Guoping Dong, Bo Peng, Jianrong Qiu, Rong Zhang, and Yi Shi  »View Author Affiliations


Optics Express, Vol. 19, Issue 27, pp. 26529-26535 (2011)
http://dx.doi.org/10.1364/OE.19.026529


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Abstract

Structural and near-infrared (NIR) emission properties were investigated in the Tm3+-Dy3+ codoped Ge-Ga-based amorphous chalcohalide films fabricated by pulsed laser deposition. The homogeneous films illustrated similar random network to the glass target according to the measurements of X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy. An 808 nm laser diode pumping generated a superbroadband NIR emission ranging from 1050 to 1570 nm and the other intense broadband NIR emission centered at ~1800 nm, which was attributed to the efficient energy transfer from Tm3+ to Dy3+ ions. This was further verified by the broad-range excitation measurements near the Urbach optical-absorption edge involved defect states. The results shed light on the potential highly integrated planar optical device applications of the codoped amorphous chalcohalide films.

© 2011 OSA

1. Introduction

Here we report on a pulsed-laser deposition (PLD) fabrication [4

4. M. Frumar, B. Frumarova, P. Nemec, T. Wagner, J. Jedelsky, and M. Hrdlicka, “Thin chalcogenide films prepared by pulsed laser doposition: new amorphous materials applicable in optoelectronics and chemical sensors,” J. Non-Cryst. Solids 352(6-7), 544–561 (2006). [CrossRef]

,26

26. J. Z. Wang, Y. Xia, Y. Shi, Z. Q. Shi, L. Pu, Z. S. Tao, and F. Lu, “1.54 μm photoluminescence emission and oxygen vacancy as sensitizer in Er-doped HfO2 films,” Appl. Phys. Lett. 91(19), 191115 (2007). [CrossRef]

] of high-quality uniform Ge-Ga-based amorphous chalcohalide films using a Tm3+-Dy3+ codoping scheme. The structures and unique NIR emission properties are explored and correlated. Both the superbroadband NIR emission with a full-width at half-maximum (FWHM) of ~400 nm and the intense NIR broadband emission (at ~1.8 μm) with a FWHM of ~200 nm are observed upon 808 nm laser diode pumping, which enables potential applications in integrated planar optical devices such as broadband planar amplifiers and tunable IR lasers. Furthermore, an energy-transfer mechanism responsible for such broadband NIR emission is proposed with the assistance of the broad-range excitation measurements. This work shows that Tm3+-Dy3+ codoping in chalcohalide films is an effective scheme to achieve the broadband NIR emission.

2. Experimental

The films were prepared by PLD from bulk chalcohalide glass target with a nominal multi-composition of 72GeS2·18Ga2S3·10CdI2 (in mol%) doped with 0.5Tm2S3·0.2Dy2S3 (in wt%). The glass was prepared by a conventional melt-quenching technique. The detailed procedure has been described elsewhere [27

27. H. T. Guo, L. Liu, Y. Q. Wang, C. Q. Hou, W. N. Li, M. Lu, K. S. Zou, and B. Peng, “Host dependence of spectroscopic properties of Dy3+-doped and Dy3+, Tm3+-codoped Ge-Ga-S-CdI2 chalcohalide glasses,” Opt. Express 17(17), 15350–15358 (2009). [CrossRef] [PubMed]

]. The obtained glass target with cylinder shape was cut into discs with thickness of ~5 mm and diameter of ~10 mm. Both surfaces of discs were polished to mirror smoothness. The chemically cleaned quartz substrate (1 × 1 cm) was loaded to the vacuum chamber (evacuated down to ~7.5 × 10−6 Torr) and positioned parallel to the glass target surface at a distance of 5 cm. The films were deposited onto the substrate at 200 °C for 30 min using a 248 nm KrF excimer laser beam (an average fluency of 2 J/cm2 and a repetition rate of 5 Hz). After deposition, the films were in situ annealed at 300 °C (below glass transition temperature) [28

28. H. T. Guo, Y. B. Zhai, H. Z. Tao, G. P. Dong, and X. J. Zhao, “Structure and properties of GeS2-Ga2S3-CdI2 chalcohalide glasses,” Mater. Sci. Eng. B 138(3), 235–240 (2007). [CrossRef]

] for 2 h to improve the film structure. The average thickness of the films was determined to be ~700 nm by a surface profiler. The surface microstructures contained uniform island-shaped grains with a mean roughness of ~1 nm, as analyzed by atomic force microscopy.

The amorphous state of the film is determined by X-ray diffraction (XRD) using a Cu line. The composition was determined by X-ray photoelectron spectroscopy (XPS) from ULVAC-PHI 5000 VersaProbe using Al source. The structure of the film was measured by Raman spectroscopy using a Raman spectrometer (Jobin-Yvon HR800) with a 514.5 nm Ar+ laser. The optical transmission spectrum was recorded using a Shimadzu UV-VIS-NIR UV-3600 spectrophotometer. The NIR emission spectrum was acquired from a Jobin-Yvon TRIAX320 spectrometer equipped with a PbSe detector by exciting the film with an 808 nm laser diode (200 mW). In addition, we also employed a Perkin-Elmer LS50B spectrophotometer equipped with an InGaAs detector by exciting the film with a 325 nm He-Cd laser, as well as an Edinburgh FLS-920 spectrometer with a xenon arc lamp equipped with a Ge detector by exciting the film at 450 and 488 nm. All the measurements were carried out at room temperature.

3. Results and discussion

Figure 1(a)
Fig. 1 (a) XRD pattern of the chalcohalide film. Inset shows the digital photographs of the film and quartz. (b) XPS survey spectrum of the chalcohalide film.
shows the XRD pattern of the chalcohalide film, indicating the amorphous state with the broad diffraction hump at ~21 degree. The film appears an orange-yellow color versus the colorless quartz substrate, as seen from the inset of Fig. 1(a). XPS analysis indicates that the film stoichiometry is similar to that of the target within the error of 5%. XPS survey spectrum is illustrated in Fig. 1(b), revealing the existence of Ge, Ga, S, Cd, and I elements except for RE ions which may escape from the detection limit of XPS.

Figure 2(a)
Fig. 2 (a) Raman spectra of the chalcohalide film and the glass target. Dashed lines are drawn as guides for the eyes. (b) Optical transmission spectrum of the chalcohalide film. Inset shows the plot of the optical gap in terms of Tauc’s law. The optical energy gap of 1.90 eV (~653 nm) is deduced by the linear extrapolation.
shows the Raman spectra of the film and target, indicating the similar random network structures since the strong Raman mode at ~348 cm−1, which is associated with the network backbone of mainly [GeS4/2] corner-sharing tetrahedral [28

28. H. T. Guo, Y. B. Zhai, H. Z. Tao, G. P. Dong, and X. J. Zhao, “Structure and properties of GeS2-Ga2S3-CdI2 chalcohalide glasses,” Mater. Sci. Eng. B 138(3), 235–240 (2007). [CrossRef]

,29

29. X. F. Wang, S. X. Gu, J. G. Yu, X. J. Zhao, and H. Z. Tao, “Structural investigations of GeS2-Ga2S3-CdS chalcogenide glasses using Raman spectroscopy,” Solid State Commun. 130(7), 459–464 (2004). [CrossRef]

], does not change. The main different feature between them is the increased intensity of ~218 cm−1 Raman mode in the film (marked with an arrow), which is most likely ascribed to the increased mixed bonds [19

19. Y. S. Xu, D. P. Chen, W. Wang, Q. Zhang, H. D. Zeng, C. Shen, and G. R. Chen, “Broadband near-infrared emission in Er3+-Tm3+ codoped chalcohalide glasses,” Opt. Lett. 33(20), 2293–2295 (2008). [CrossRef] [PubMed]

], such as I-Tm-S and Tm-A (A= I, S)-Dy. Cd-S bonds are also partially responsible for such a mode [29

29. X. F. Wang, S. X. Gu, J. G. Yu, X. J. Zhao, and H. Z. Tao, “Structural investigations of GeS2-Ga2S3-CdS chalcogenide glasses using Raman spectroscopy,” Solid State Commun. 130(7), 459–464 (2004). [CrossRef]

]. The mode at ~276 cm−1 is mainly associated with the [GaS3/2I]- units, coming from the broken [GaS4/2]- structural units by I- [30

30. T. H. Lee, Y. K. Kwon, and J. Heo, “Local structure and its effect on the oscillator strengths and emission properties of Ho3+ in chalcohalide glasses,” J. Non-Cryst. Solids 354(27), 3107–3112 (2008). [CrossRef]

,31

31. J. H. Song and J. Heo, “Effect of CsBr addition on the emission properties of TM3+ ion in Ge-Ga-S glass,” J. Mater. Res. 21(09), 2323–2330 (2006). [CrossRef]

]. Based on these facts, it is reasonable to conclude that there are more abundant defect states in the film due to the broken network and hosted RE ions nearby [30

30. T. H. Lee, Y. K. Kwon, and J. Heo, “Local structure and its effect on the oscillator strengths and emission properties of Ho3+ in chalcohalide glasses,” J. Non-Cryst. Solids 354(27), 3107–3112 (2008). [CrossRef]

,31

31. J. H. Song and J. Heo, “Effect of CsBr addition on the emission properties of TM3+ ion in Ge-Ga-S glass,” J. Mater. Res. 21(09), 2323–2330 (2006). [CrossRef]

], leading to unique emission properties. The vibrational modes at ~376, 420, and 492 cm−1 arise from the [GeS4/2] edge-sharing tetrahedra, Ge-S-Ge bonds, and short S-S chains, respectively [28

28. H. T. Guo, Y. B. Zhai, H. Z. Tao, G. P. Dong, and X. J. Zhao, “Structure and properties of GeS2-Ga2S3-CdI2 chalcohalide glasses,” Mater. Sci. Eng. B 138(3), 235–240 (2007). [CrossRef]

,29

29. X. F. Wang, S. X. Gu, J. G. Yu, X. J. Zhao, and H. Z. Tao, “Structural investigations of GeS2-Ga2S3-CdS chalcogenide glasses using Raman spectroscopy,” Solid State Commun. 130(7), 459–464 (2004). [CrossRef]

]. It should be noted that the formation of [GaS3/2X]- (X = Cl, Br, I) units which have the lower phonon energy and the formation of mixed bonds which suppress the cross relaxation between each RE ion can both enhance the emission properties of RE ions to some extent [19

19. Y. S. Xu, D. P. Chen, W. Wang, Q. Zhang, H. D. Zeng, C. Shen, and G. R. Chen, “Broadband near-infrared emission in Er3+-Tm3+ codoped chalcohalide glasses,” Opt. Lett. 33(20), 2293–2295 (2008). [CrossRef] [PubMed]

,31

31. J. H. Song and J. Heo, “Effect of CsBr addition on the emission properties of TM3+ ion in Ge-Ga-S glass,” J. Mater. Res. 21(09), 2323–2330 (2006). [CrossRef]

].

The typical optical transmission spectrum of the film is shown in Fig. 2(b). Obviously, the film is transparent with transmittance as high as 70% from 600 nm to the NIR region. The interference fringes at the transparent wavelengths are characteristic in film form [2

2. A. P. Caricato, M. D. Sario, M. Fernandez, M. Ferrari, G. Leggieri, A. Luches, M. Martino, M. Montagna, F. Prudenzano, and A. Jha, “Chalcogenide glass thin film waveguides deposited by excimer laser ablation,” Appl. Surf. Sci. 208–209, 632–637 (2003). [CrossRef]

]. The intrinsic absorption edge is of Urbach type [32

32. N. F. Mott and E. A. Davis, Electronic Processes in Non-Crystalline Materials (Clarendon, Oxford, 1979).

] and located at ~450-600 nm. The optical bandgap (Egopt) is deduced to be 1.90 eV (~653 nm) by extrapolating the linear part of (αhν)1/2 curve to the abscissa () according to Tauc’s law [33

33. J. Tauc, Amorphous and Liquid Semiconductors (Plenum, New York, 1974).

], in which α is the absorption coefficient and () is the energy of light, as shown in the inset of Fig. 2(b). The region between Urbach edge and optical bandgap is labeled as the weak absorption tail due to the absorption by impurities and defects in the film [33

33. J. Tauc, Amorphous and Liquid Semiconductors (Plenum, New York, 1974).

].

In order to clarify the NIR emission mechanism of Tm3+-Dy3+ codoped chalcohalide film, we have also performed the pumping experiment using the variable-wavelength scheme. The emission spectra are shown in Fig. 3(b). It is found that pumping light with wavelengths ranging from 325 to 488 nm, covering the Urbach absorption edge of the film, can all excite the Tm3+ or Dy3+ characteristic intra-4f-shell transitions at ~1230 and 1330 nm, corresponding to the Tm3+: 3H53H6 and Dy3+: 6H9/2 + 6F11/26H15/2 transitions, respectively. In addition, an intense incomplete emission peaked at 1825 nm due to Tm3+: 3F43H6 transition is observed when excited at 325 nm which is constrained by the upper limit of the InGaAs detector at 1900 nm. These NIR emission lines are symmetric and originate from the energy-transfer process from the film to the RE ions, similar to the case in RE-doped chalcogenide glasses [34

34. S. Q. Gu, S. Ramachandran, E. E. Reuter, D. A. Turnbull, J. T. Verdeyen, and S. G. Bishop, “Novel broad-band excitation of Er3+ luminescence in chalcogenide glasses,” Appl. Phys. Lett. 66(6), 670–672 (1995). [CrossRef]

,35

35. S. G. Bishop, D. A. Turnbull, and B. G. Aitken, “Excitation of rare earth emission in chalcogenide glasses by broadband Urbach edge absorption,” J. Non-Cryst. Solids 266–269, 876–883 (2000). [CrossRef]

]. The schematic mechanism resulting in such broad-range excitations is illustrated in Fig. 4(a)
Fig. 4 Schematic energy-level diagrams, showing the energy-transfer mechanism (a) between the chalcohalide film and RE ions under 325-488 nm pumping and (b) between Tm3+ and Dy3+ under 808 nm pumping. The filled and open circles denote electrons and holes, respectively. The NIR emission bands are also indicated in the diagrams with the units of nm. ET: energy transfer.
. Firstly the 325-488 nm pumping leads to the light absorption in the Urbach edge and then excites an electron-hole pair in the film. Then the defect states capture the resultant hole, undergo a lattice relaxation due to the changed charge state, and move deeper into the gap. Finally, the recombination of the hole with the bound electron non-radiatively transfers energy to the nearby RE ions, giving rise to the intra-4f transitions of Tm3+ and Dy3+. These broad-range excitations may enable a variety of pumping schemes for planar optical devices [34

34. S. Q. Gu, S. Ramachandran, E. E. Reuter, D. A. Turnbull, J. T. Verdeyen, and S. G. Bishop, “Novel broad-band excitation of Er3+ luminescence in chalcogenide glasses,” Appl. Phys. Lett. 66(6), 670–672 (1995). [CrossRef]

,35

35. S. G. Bishop, D. A. Turnbull, and B. G. Aitken, “Excitation of rare earth emission in chalcogenide glasses by broadband Urbach edge absorption,” J. Non-Cryst. Solids 266–269, 876–883 (2000). [CrossRef]

].

4. Conclusion

In conclusion, we have fabricated the high-quality Tm3+-Dy3+ codoped amorphous chalcohalide films by pulsed laser deposition. The film shows the remarkable superbroadband (from 1050 to 1570 nm) NIR emission and the intense broadband NIR emission centered at ~1800 nm, covering the whole low-loss wavelength region of silica optical fibers. This is contributed by the Tm3+ sensitization and the efficient energy-transfer process from Tm3+ to Dy3+, which is verified by the broad-range excitation near Ulbach optical-absorption edge. The results make the codoped chalcohalide films as promising candidates for developing highly integrated planar optical devices, such as broadband planar amplifiers and tunable IR lasers.

Acknowledgments

This work was supported by the National Natural Science Foundation of China (Grant Nos. 10904100, 61176088, 60990311, 60990314, 10876009, and 60807034), the Natural Science Foundation of Jiangsu Province (Grant No. BK2011557), the Fundamental Research Funds for the Central Universities, and the National Key Projects for Basic Research of China (Grant No. 2011CB301900).

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3.

J. A. Frantz, L. B. Shaw, J. S. Sanghera, and I. D. Aggarwal, “Waveguide amplifiers in sputtered films of Er3+-doped gallium lanthanum sulfide glass,” Opt. Express 14(5), 1797–1803 (2006). [CrossRef] [PubMed]

4.

M. Frumar, B. Frumarova, P. Nemec, T. Wagner, J. Jedelsky, and M. Hrdlicka, “Thin chalcogenide films prepared by pulsed laser doposition: new amorphous materials applicable in optoelectronics and chemical sensors,” J. Non-Cryst. Solids 352(6-7), 544–561 (2006). [CrossRef]

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V. Nazabal, P. Nemec, A. M. Jurdyc, S. Zhang, F. Charpentier, H. Lhermite, J. Charrier, J. P. Guin, A. Moreac, M. Frumar, and J. L. Adam, “Optical waveguide based on amorphous Er3+-doped Ga-Ge-Sb-S(Se) pulsed laser doposited thin films,” Thin Solid Films 518(17), 4941–4947 (2010). [CrossRef]

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M. Y. Peng, J. R. Qiu, D. P. Chen, X. G. Meng, I. Yang, X. W. Jiang, and C. S. Zhu, “Bismuth- and aluminum-codoped germanium oxide glasses for super-broadband optical amplification,” Opt. Lett. 29(17), 1998–2000 (2004). [CrossRef] [PubMed]

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M. A. Hughes, T. Akada, T. Suzuki, Y. Ohishi, and D. W. Hewak, “Ultrabroad emission from a bismuth doped chalcogenide glass,” Opt. Express 17(22), 19345–19355 (2009). [CrossRef] [PubMed]

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H. T. Sun, F. Shimaoka, Y. Miwa, J. Ruan, M. Fujii, J. R. Qiu, and S. Hayashi, “Sensitized superbroadband near-IR emission in bismuth glass/Si nanocrystal superlattices,” Opt. Lett. 35(13), 2215–2217 (2010). [CrossRef] [PubMed]

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J. Ruan, G. P. Dong, X. F. Liu, Q. Zhang, D. P. Chen, and J. R. Qiu, “Enhanced broadband near-infrared emission and energy transfer in Bi-Tm-codoped germanate glasses for broadband optical amplification,” Opt. Lett. 34(16), 2486–2488 (2009). [CrossRef] [PubMed]

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B. Zhou, H. Lin, B. J. Chen, and E. Y. B. Pun, “Superbroadband near-infrared emission in Tm-Bi codoped sodium-germanium-gallate glasses,” Opt. Express 19(7), 6514–6523 (2011). [CrossRef] [PubMed]

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Y. S. Xu, D. P. Chen, W. Wang, Q. Zhang, H. D. Zeng, C. Shen, and G. R. Chen, “Broadband near-infrared emission in Er3+-Tm3+ codoped chalcohalide glasses,” Opt. Lett. 33(20), 2293–2295 (2008). [CrossRef] [PubMed]

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J. Z. Wang, Y. Xia, Y. Shi, Z. Q. Shi, L. Pu, Z. S. Tao, and F. Lu, “1.54 μm photoluminescence emission and oxygen vacancy as sensitizer in Er-doped HfO2 films,” Appl. Phys. Lett. 91(19), 191115 (2007). [CrossRef]

27.

H. T. Guo, L. Liu, Y. Q. Wang, C. Q. Hou, W. N. Li, M. Lu, K. S. Zou, and B. Peng, “Host dependence of spectroscopic properties of Dy3+-doped and Dy3+, Tm3+-codoped Ge-Ga-S-CdI2 chalcohalide glasses,” Opt. Express 17(17), 15350–15358 (2009). [CrossRef] [PubMed]

28.

H. T. Guo, Y. B. Zhai, H. Z. Tao, G. P. Dong, and X. J. Zhao, “Structure and properties of GeS2-Ga2S3-CdI2 chalcohalide glasses,” Mater. Sci. Eng. B 138(3), 235–240 (2007). [CrossRef]

29.

X. F. Wang, S. X. Gu, J. G. Yu, X. J. Zhao, and H. Z. Tao, “Structural investigations of GeS2-Ga2S3-CdS chalcogenide glasses using Raman spectroscopy,” Solid State Commun. 130(7), 459–464 (2004). [CrossRef]

30.

T. H. Lee, Y. K. Kwon, and J. Heo, “Local structure and its effect on the oscillator strengths and emission properties of Ho3+ in chalcohalide glasses,” J. Non-Cryst. Solids 354(27), 3107–3112 (2008). [CrossRef]

31.

J. H. Song and J. Heo, “Effect of CsBr addition on the emission properties of TM3+ ion in Ge-Ga-S glass,” J. Mater. Res. 21(09), 2323–2330 (2006). [CrossRef]

32.

N. F. Mott and E. A. Davis, Electronic Processes in Non-Crystalline Materials (Clarendon, Oxford, 1979).

33.

J. Tauc, Amorphous and Liquid Semiconductors (Plenum, New York, 1974).

34.

S. Q. Gu, S. Ramachandran, E. E. Reuter, D. A. Turnbull, J. T. Verdeyen, and S. G. Bishop, “Novel broad-band excitation of Er3+ luminescence in chalcogenide glasses,” Appl. Phys. Lett. 66(6), 670–672 (1995). [CrossRef]

35.

S. G. Bishop, D. A. Turnbull, and B. G. Aitken, “Excitation of rare earth emission in chalcogenide glasses by broadband Urbach edge absorption,” J. Non-Cryst. Solids 266–269, 876–883 (2000). [CrossRef]

36.

J. Heo, W. Y. Cho, and W. J. Chung, “Sensitizing effect of Tm3+ on 2.9 μm emission from Dy3+-doped Ge25Ga5S70 glass,” J. Non-Cryst. Solids 212(2-3), 151–156 (1997). [CrossRef]

OCIS Codes
(160.5690) Materials : Rare-earth-doped materials
(300.6280) Spectroscopy : Spectroscopy, fluorescence and luminescence

ToC Category:
Materials

History
Original Manuscript: September 6, 2011
Revised Manuscript: November 17, 2011
Manuscript Accepted: November 28, 2011
Published: December 13, 2011

Citation
Senlin Yang, Xuefeng Wang, Haitao Guo, Guoping Dong, Bo Peng, Jianrong Qiu, Rong Zhang, and Yi Shi, "Broadband near-infrared emission in Tm3+-Dy3+ codoped amorphous chalcohalide films fabricated by pulsed laser deposition," Opt. Express 19, 26529-26535 (2011)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-19-27-26529


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References

  1. S. Ramachandran and S. G. Bishop, “Excitation of Er3+ emission by host glass absorption in sputtered films of Er-doped Ge10As40Se25S25 glass,” Appl. Phys. Lett.73(22), 3196–3198 (1998). [CrossRef]
  2. A. P. Caricato, M. D. Sario, M. Fernandez, M. Ferrari, G. Leggieri, A. Luches, M. Martino, M. Montagna, F. Prudenzano, and A. Jha, “Chalcogenide glass thin film waveguides deposited by excimer laser ablation,” Appl. Surf. Sci.208–209, 632–637 (2003). [CrossRef]
  3. J. A. Frantz, L. B. Shaw, J. S. Sanghera, and I. D. Aggarwal, “Waveguide amplifiers in sputtered films of Er3+-doped gallium lanthanum sulfide glass,” Opt. Express14(5), 1797–1803 (2006). [CrossRef] [PubMed]
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