IEEE TRANSACTIONS ON NUCLEAR SCIENCE, VOL. 54, NO. 4, AUGUST 2007 1115 Low-Dose Radiation-Induced Attenuation at InfraRed Wavelengths for P-Doped, Ge-Doped and Pure Silica-Core Optical Fibres Elise Regnier, Ivo Flammer, Sylvain Girard, Frans Gooijer, Frank Achten, and Gerard Kuyt Abstract—Exposing optical silica fibers to radiative environments leads to an increase of fiber attenuation. This gamma-sensitivity of the fibers is strongly wavelength dependent. Many papers already mentioned the strong Radiation-Induced Attenuation (RIA) in the UV and Visible ranges, which is explained by radiation-induced defects absorbing in these spectral ranges. However, 1000 nm) is less the origin of RIA at longer wavelengths ( clear. An exception is phosphorous-doped fibers for which P1 defects absorbing around 1700 nm have already been highlighted. For fibers with no phosphorus, the RIA at Near-InfraRed (NIR) wavelengths is usually assumed to be small as it results from the UV-visible absorption tail, which decreases with increasing wavelength. In this paper, we study three prototype silica based optical fibers and show that the RIA does not monotically decrease with increasing wavelength, highlighting RIA-contributions having their origins at NIR-wavelengths. We show that these NIR-absorbing defects are generally the main contributor to RIA at telecommunication wavelengths (1310 nm and 1550 nm), the impact of UV-visible absorption tail being secondary only. The nature of defects involved in these NIR absorptions depends on fiber composition. For fibers with no phosphorous, we propose Self Trapped Hole defects (STH) as origin. Index Terms—Fiber, infrared, pure and doped silica, radiation. I. INTRODUCTION L IGHT transmission in optical fibers exposed to radiative environment is strongly affected by the formation of point defects in silica network. The nature of radiation-induced defects depends mainly on glass composition, but also on other parameters like glass thermal history or residual stress [1]. Each defect has specific absorption properties, growth and recovery kinetics. The Radiation-Induced Attenuation (RIA) therefore depends on many parameters: fiber composition, irradiation conditions (dose-rate, temperature, total dose) and operating conditions (wavelength, injected power, measurements under radiation or after a few weeks during which unstable defects anneal). Thus the correct choice of a radiation resistant fiber depends on the irradiation conditions and the fiber’s working conditions. Manuscript received October 6, 2006; revised January 26, 2007. This work was supported by Draka Comteq. E. Regnier and I. Flammer are with Draka Comteq France, 91460 Marcoussis, France (e-mail: [email protected]; [email protected]). S. Girard is with the CEA DIF, 91680 Bruyères-le-Châtel, France (e-mail: [email protected]). F. Gooijer, F. Achten, and G. Kuyt are with Draka Comteq Fibre BV, 5651 Eindhoven, The Netherlands (e-mail: [email protected]; frank.achten@ draka.com; [email protected]). Digital Object Identifier 10.1109/TNS.2007.894180 Long-Term Radiation-Induced Attenuation (i.e., RIA that remains even a long time after the end of the radiation, when all the unstable defects have been annealed) has been widely studied over the past few decades, and it is now a well-known fact that RIA generally increases with shorter wavelengths, as many radiation-induced defects absorb in the ultraviolet (UV) and visible ranges. These UV-visible absorbing defects have already been studied in detail [2]–[4]: Ge(1), Ge(2), GEC, GeE’ with regard to Germanium-related defects, POHC, P2 and P4 defects with regards to Phosphorus-related defects, and also NBOHC, POR, SiE’ and Self-Trapped-Hole (STH) defects. Absorption bands of these defects are located from 195 nm (GeE’) up to Visible wavelengths (550 nm for the POHC, 630 nm for the NBOHCs, 540 nm, 660 nm and 760 nm for the STHs). Hownm), opever, at Near InfraRed (NIR) wavelengths ( tical fibers sometimes exhibit RIA increasing with wavelength [5], [6]. Such behavior reveals the existence of absorption bands centered in the NIR. Contrary to UV-defects, these defects are not so well-known, except for P-doped fibers, in which a NIR -induced absorption has already been attributed to P1 defects [7]. For fibers of Pure Silica Core Fiber (PSCF) type (pure or fluorine-doped silica cores), a broad absorption band centered near 1600–1700 nm has been attributed to STH defects [8], [9]. However, these defects are thought to exist only at low temperatures [8]. In [10], Griscom proposes that STH defects may exist at room temperature and may therefore lead to InfraRed absorption excesses. In Ge-doped fibers, the existence of a Long-Term NIR-RIA has been shown in [5] and [6], as irradiated Ge-doped single-mode fibers (SMF) and multimode fibers (MMF) showed very broad -induced bands centered around 2050 nm and at a wavelength 2500 nm, respectively. To our knowledge, neither of these two bands have been identified yet. The purpose of this paper is to clarify the Long-Term NIRpart of the RIA, as well as to quantify and to compare it to the UV-visible contribution. We compare the RIA spectra in three prototype silica-based fibers gamma-irradiated at low dose levels (from 5 Gy to 100 Gy) and with three different core compositions: one is P-doped, the second one is of PSCF type, and the last one is Ge-doped. We show that for telecommunication applications it is the NIR-absorption band which mainly determine the RIA level. II. EXPERIMENTAL PROCEDURE For this study, three prototype singlemode fibers were realized: Fiber1, Fiber2 and Fiber3. Fiber1 is P-doped in core wt%) and Fiber3 Ge-doped ( wt%). Fiber2 is of PSCF ( 0018-9499/$25.00 © 2007 IEEE 1116 IEEE TRANSACTIONS ON NUCLEAR SCIENCE, VOL. 54, NO. 4, AUGUST 2007 The sum of these three components results in a minimumRIA window around 1000 nm for Fiber1, 1100–1200 nm for Fiber2, and 1200–1300 nm for Fiber3. Fig. 1 also confirms the well-known very poor radiation-resistance of P-doped fibers compared to Ge-doped and undoped silica fibers over the whole spectral range [1], [4], [11]: despite the low gamma-dose (5 Gy) applied to the P-doped fiber compared to the dose applied to the Ge-doped and undoped fibers (100 Gy), the RIA is much higher for the P-doped fiber. IV. DISCUSSION A. Method to Extract the NIR-RIA Contribution Fig. 1. Normalized RIA spectra for the P-doped fiber (after 5 Gy), the Ge-doped fiber, and the undoped fiber (after 100 Gy). type and contains only fluorine to lower its refractive index profile. The three fibers have been made using CVD technique. We conducted the irradiation experiments within the CEA, Bruyères-le-Chatel, France, using a Co source at room temperature. We irradiated a few kilometers of each fiber. The P-doped fiber (Fiber1) has been irradiated at a total dose of 5 Gy and Fiber2 and Fiber3 at 100 Gy. We performed spectral attenuation measurements both before and after the gamma-exposure. Attenuation measurements performed after the radiation have been made a few weeks after the irradiation, which means that most of the unstable defects were already annealed. These attenuation measurements were performed at room temperature, from 450 nm up to maximum 2100 nm. For NIR-measurements, we took care of minimizing bending losses by zero-stress spooling of the fiber. Uncertainty of the attenuation mea% for 800 nm (home-made surements is maximum nm (optimized Bentham-bench). For bench) and nm (commercial PK2200 apparatus), dB/km. attenuation uncertainty is smaller: III. EXPERIMENTAL RESULTS Fig. 1 shows the normalized Radiation-Induced Attenuation spectra for the three fibers studied. Normalization has been made so that RIA at 1550 nm for the undoped fiber is equal to 1 dB/km. Note that the largest wavelength up to which we could determine the RIA spectra depends on the RIA level. Indeed, due to the measurement uncertainty on attenuation % for spectra both before and after the radiation exposure ( nm) and due to the high attenuation level of silica at long wavelengths (higher than 7 dB/km for nm), only RIA larger than 1.7 dB/km can be measured for these wavelengths. This explains why RIA could not be determined nm for Fiber2 and Fiber3. Because RIA of Fiber1 for is larger, we could measure it up to 2100 nm. One can see from Fig. 1 that for all three types of fibres, RIA curves result from three main contributions: — an UV-absorption tail that strongly increases with decreasing wavelength, — absorption bands located in the Visible range (especially strong for Fiber1 and Fiber2), — an IR-contribution that increases with increasing wavelength. In order to get more information on the NIR-part of the RIA, we have extracted the NIR-contribution by subtracting all the UV and visible contributions from the RIA-spectra. To do that, we fitted the radiation-induced visible bands with Gaussian band shapes, as widely assumed for defects in inhomogeneous solids like vitreous silica (see for example [7], [12]). Local electrical fields existing in the disordered silica matrix indeed impact the electronical environment of absorbing defects, and therefore impact their absorption energy, shifting it to lower or upper energies with a certain distribution. Gaussian functions with quite large width generally well fit the resulting absorption bands around the maximum of absorption. In addition to these bands located in the visible range, we chose to consider an absorption contribution of an exponential form , assuming that this contribution includes the sum of all the long absorption tails of radiation-induced defects absorbing in the VUV-UV range. The values of C and K depend on both the total dose and the fiber type. The fit of this UV contribution has been performed based on RIA values around both 450 nm and 1100 nm, i.e., where the UV-tail is predominant. Even if the fits of the UV and visible contributions are quite raw, this allowed us to determine the main contribution of the RIA (UV or NIR contribution) at both 1310 and 1550 nm (uncertainty on the contribution smaller %). Having fitted the UV-contribution with another than wavelength dependency could have led to slightly larger uncertainty, but would not have changed the conclusion concerning the main RIA contribution. B. Phosphorus-Doped Fibers For the P-doped fiber, RIA spectrum can be fitted by a UV-tail and a sum of two Gaussian curves centered around 540 nm (attributed to POHC defects [7]) and 1620 nm (attributed to P1 defects [7]) (see Fig. 2). From Fig. 2, one can see that at telecom wavelengths, RIA of P-doped fibers is due almost entirely to P1 defects: at both, 1310 nm and 1550 nm, radiation-induced absorption due to P1-absorption band represents the main origin of RIA, with more than 80% and 90% of the total RIA, respectively. We deduce from these RIA decomposition that the P1 band is well fitted by a Gaussian function, with a maximum located eV ( nm) and a FWHM of at eV. These values agree with literature data that state the band maximum of P1 defects between 0.76 and 0.79 eV [7] and a FWHM from 0.26 to 0.35 eV [7]. Our very good precision REGNIER et al.: LOW-DOSE RADIATION-INDUCED ATTENUATION AT INFRARED WAVELENGTHS Fig. 2. Normalized RIA (after 5 Gy) of the P-doped fiber can be fitted by a UV-tail, and two absorption bands located around 540 nm and 1620 nm. Fig. 3. Normalized RIA (after 100 Gy) decomposition for Fiber2: we can see a UV-tail, at least two absorption bands located in the Visible range (around 650 nm and 750 nm), and one absorption band in the NIR. on P1 peak position and peak width is due to the fact that at such long wavelengths, the RIA is almost exclusively due to P1-defects and because we took into account the wavelength dependency of the mode power fraction in the P-doped part of the fiber (as already suggested in [13]). The calculation of this power fraction is based on Maxwell propagation equations applied to a cylindrical dielectrical waveguide in which the usual weakly guiding approximation was made. Features of the waveguide are determined by measuring the refractive index profile of the preform. Not taking this effect into account would have led to an error on the peak maximum of about 90 nm (maximum would have been found around 1530 nm instead of 1620 nm). In addition to that, the shape of the band-fit would also have been somewhat distorted, with an underestimation of P1-contribution at long wavelengths. C. Undoped Fibers The RIA-decomposition for Fiber2 is shown in Fig. 3. It allowed us to highlight the existence of absorption bands located in the visible range (at least two bands around 650 nm and 750 nm) and a broad NIR-absorption band, which is responsible for more than 90% of total RIA at 1550 nm, and more than 75% of total RIA at 1310 nm. Gamma-sensitivity of the undoped fiber at telecommunication wavelengths thus mainly results from this NIR-band. By fitting this band by a Gaussian function, we find a peak maximum around 1800 nm (about 0.7 eV, eV) (see Fig. 3). 1117 Fig. 4. Intensity of the NIR-absorption band attributed to STH defects. Data at 77 K, 130 K, 145 K, and 160 K are extracted from [1]. Data at 300 K has been obtained in this study. Because this band maximum is very close to that of the absorption band attributed to STH defects by Chernov et al. [11], we think that this NIR-band is related to STHs. In addition to that, the presence of a second absorption band located around 750 nm, which is characteristic for STH defects too, tends to confirm the presence of these defects. However, the presence of STHs in our fiber (irradiated and measured at room temperature) is surprising as STHs are known to be unstable at room temperature. Up to now, the NIR-band attributed to STHs has been observed up to 160 K only [10], but not at higher temperatures. Chernov et al. showed that this NIR-band decreases when increasing temperature. As shown in Fig. 4, RIA-measurements performed on our undoped fiber irradiated at the same total dose as that used by Chernov show that the NIR-band intensity is more than two orders of magnitude smaller than that measured at low temperature in [10]. The fact that we still observe STH, even at room temperature, is therefore probably due to our very high measurement sensitivity obtained by using fibers of several km in length (note that Chernov et al. used fiber samples of only 4 m in length). This therefore tends to show that STH defects exist at room temperature, but at very extremely low contents. The appearance of STHs in pure silica tends to show that their formation is related to the glass matrix properties. To reduce the formation of these defects, Yamaguchi et al. [14] propose to reduce the glass disorder. D. Ge-Doped Fibers For the Ge-doped fibre, the RIA spectrum suggests the existence of absorption structures between 550 nm and 850 nm, and a very broad absorption band having its origin in the NIR range, at nm (see Fig. 5). With the available data ( nm), we can’t have much precision about the exact location of this band. Measurements performed after higher dose would be needed to determine the exact location. Despite this low precision, we can clearly see that the impact of this NIRband at 1310 nm is not so strong as for the P-doped and undoped fibers: at this wavelength, the NIR-band contribution is secondary only (around 40%). However, at 1550 nm, the NIR-contribution becomes bigger and even the main contribution, with more than 80% of the total RIA. The origin of this NIR absorption band might be linked to some Ge-impacted STH defects, with optical properties slightly different from “regular” STH 1118 IEEE TRANSACTIONS ON NUCLEAR SCIENCE, VOL. 54, NO. 4, AUGUST 2007 Fig. 5. Normalized RIA (after 100 Gy) decomposition for the Ge-doped fiber: we can see the presence of the UV-absorption tail, some absorption bands in the Visible range, and a broad band centered in the NIR range. defects. Such defects have actually already been mentioned in literature. For example, Sasajima showed by calculation that Ge-defects called Small Polaron defects (SP(Ge)) are similar to STH defects, but have slightly different optical absorption properties: he measured an STH-absorption band around 2.6 eV, and an absorption band related to SP(Ge) around 2.2 eV [15]. Also Pacchioni published some calculations on Ge-Lone-Pair showing that such deCenter with a trapped hole fects have energies similar to that of STHs [16]. At last, Nishii et al. [17], [18] show by ESR measurements that STH defects also exist in Ge-doped silica irradiated at low temperature. We thus propose that the NIR-band observed in our Ge-doped fiber is due to some STH species, whose absorption properties could be slightly changed due to the presence of Germanium atoms in their neighborhood. Comparing the RIA data of Fiber 2 and Fiber 3, we see that the contribution of the NIR-absorption band at 1310 nm and 1550 nm is slightly lower in Ge-doped fibres than in fibres with no Ge. This can be explained firstly by the fact that the UV-absorption tail is somewhat stronger in the Ge doped fiber, and secondly because the NIR-absorption band in Ge-doped SMF is centered at higher wavelengths than the NIR-band in undoped SMF. For higher doses (up to 100 000 Gy), we observed that UV-tail and NIR-contribution increase much more in the Ge-doped fibre than in the undoped fiber. In this case, RIA for Ge-doped fibers is larger over the whole studied wavelength range (from 450 nm up to 2000 nm). At such high doses, fibers with no Ge should thus be preferred to Ge-doped fibers. At last, we can note that our results differ from measurements performed on erbium-doped fibers, where the UV absorption tail seems to be the main contribution, even at NIR wavelengths [19]. Erbium-doped fibers however usually show much higher RIA values than fibers studied here [20]. The strong UV-contribution can be explained by the presence of specific dopants like Aluminium [21]. Also the role of Erbium ions is discussed by certain authors [20]. V. CONCLUSION We have seen in this paper that attenuation properties of optical fibers exposed to radiative environments are impacted by the formation of defects absorbing not only in the UV-visible range, but in the NIR range too. We even show that this NIR- contribution mainly determines the RIA level at both standard telecommunication wavelengths (1310 nm and 1550 nm). This is the case for all three studied fibers: the P-doped silica fiber, the Ge-doped silica fiber and the undoped silica fiber. It is therefore very important to be aware of the existence of these bands and to study their properties in more details. In fibers with no P, we propose that the NIR-absorption bands are related to STH species. Note that such defects are likely to exist not only in silica fibers exposed to radiations, but also in all today’s technologies based on silica material and exposed to radiative environments. 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