100 OPTICS LETTERS / Vol. 18,No. 19 / October 1, 1990 Optical-fiber temperature sensor based on upconversion-excited fluorescence H. Berthou Swiss Center for Electronics and Microtechnology, Research and Development CH2000 Neuchotel7, Switzerland C.K. Jorgensen Department of Inorganic and Applied Chemistry, Sciences Il, University of Geneva, CH 1211 Geneva 4, Switzerland Received March 12, 1900; accepted june 25,1090 ‘The codoping of a heavy-metal fluoride glass by two rare-earth ions, erbium and ytterbium, permits the semicon: Guctor laser infrared excitation of two visible neighboring fluorescence lines of erbium by upconversion, the Intensity ratio of which is single variable function of temperature. Optical-fiber temperature sensors based on fluores- cence have been around for a few years.’ Most make use of the temperature dependence of the fluorescence decay time?’ or of a semiconductor absorption edge.* Sensors applying such a principle were, however, shown not to give a temperature accuracy better than a fow degrees.” There are numerous applications in which such an error is acceptable if the whole system has a low cost and long life. While still based on the temperature dependence of fluorescence, the ap- proach proposed and demonstrated here is a judicious combination of a glassy host material and rare-earth dopants that uses two fluorescence lines of a Boltz- mannian population excited by means of a semicon- ductor-laser-induced upconversion. ‘The signal processing of a fluorescent sensor is con- siderably simplified if, instead of requiring a time- resolved measurement, the temperature information can be given as the ratio of two light intensities. Two conditions must be met: the ratio is an intrinsic func- tion of temperature alone, and the ratio of the two optical signals is conveyed down the fiber regardless of variations of the excitation source level and the fiber length and possible fluctuations of transmission. ‘The first condition is fulfilled by the 2Hiyyi2 and ‘Ss. levels of erbium that fluoresce at 520 and 650 nm, respectively. The noticeable feature of this pair of excited levels is that they are close to each other (ener- gy gap of ~800 cm), permitting the 7Hiy/12 level to be populated from the “Sy by thermal agitation (kT ~ 200 cm"), The temperature T in kelvins can there- fore be expressed from the ratio R of the two fluores- cence intensities Isa and Isso, 1/T = (k/AB)[In(C) — In(R)], a where R = I520/Isso, # is the Boltzmann constant, AE is the energy gap between the two excited levels, and Cis a constant depending on the two level lifetimes, their electronic weight, and the detector sensitivites.” R increases with temperature as the °1/12 fluorescent level is increasingly populated from the ‘Syjz. ‘The second condition, which concerns the fiber (0146-9592/90/191100-0382.00/0 transmission insensitivity, is also satisified, as the ef- fect of bends and microbends and the fluctuations thereof on the spectral loss curve of the fiber simply amounts to an amplitude shift. The detected power ratio therefore remains unaffected; this is even more so here as the spectral lines are close to each other. For practical use, the rare-earth ions should not. be part of an oxide glass as nonradiative transitions ‘quench partly (in germanate or tellurite glasses)’ or even totally (in silicate glass) the fluorescence in this part of the spectrum.® A much better excitation effi- ciency is expected from fluoride glasses, which show less-energetic phonons, and therefore more fluores- cence efficiency,° and also permit much higher concen- trations of rare-earth ions as these are well substituted for one of the glass-forming ions.!° ‘The Hiyyi2 and 4837p fluoresence lines can be effi- ciently excited in the absorption line centered at 485 nm, However, all available sources of sufficiently high optical power in the blue are not practical in real systems for cost and lifetime reasons. The desirable system solution is a semiconductor laser excitation that uses some kind of two-photon absorption. The codoping of a glass matrix by a judicious pair of rare- earth ions permits in principle the desired upconver- sion.!! The excitation of the two fluorescent levels of erbium through such a process can be performed by the codoping of ytterbium,*"? the spectrum of which exhibits the interesting feature of a single broad ab- sorption line centered at ~975 nm. As depicted sche- matically in Fig. 1, the direct excitation of the *F;j2 ytterbium level by absorption of two IR photons fol- lowed by energy transfer to the ‘Ti1 level of erbium promotes this last state to the “Fy, which, by a fast, nonradiative decay, populates the ‘Sz erbium level. Our first experiments were performed on erbium- doped germanate glasses. Exciting them with the 488-nm line of an argon laser did not show measurable green fluorescence. Heavy-metal fluoride glasses did show much better efficiency. Among the many possi- ble types, the best choice was BIZYT glass (made of barium, indium, zinc, yttrium, and thorium fluo- © 1990 Optical Society of AmericaOctober 1, 1990 / Vol. 15,No.18 / OPTICSLETTERS 1101 Fig. 1. Upconversion process between ytterbium and erbi- ‘um|evels. TE, energy transfer. Fig.2. | Fluorescence intensity ratio versus temperature for a ZBLA fluoride optical fiber, doped with 1% erbium, under direct absorption at 488 nm (argon laser). Tides!9), because of its broader transmittivity range, high melting and crystallization temperatures, low sensitivity to humidity, ability to be fibered, and hav- ing in a bulk form high fluorescence signal amplitudes. ‘To improve the fluorescence capture, the transducer material was shaped in a multimode fiber form (ZBLA glass) by Le Verre Fluoré, Vern/Seiche, France, and butt coupled to the end of a 200-um-core/300-um- cladding silica fiber lead that was 3-25 m long. Figure 2 shows the temperature dependence of the fluorescence intensity ratio R for such seven sensor elements with a 10-mW argon-laser excitation. ‘The backscattered fluorescent signal amplitudes were syn- chronously detected by means of a lock-in amplifier. "The exponential dependence on temperature in Eq. (1) was assessed by attempting a best fit with the experimental curves, which gave values for C and AE of 5.57 £ 0.22 and 776 + 11 cm", respectively, in agreement with previous results.” A maximum de ation of 2 K was found over the whole temperature range (20-200°C). ‘The next experiment was carried out with ytterbi- um-erbium codoped fluoride glass samples in order to assess the feasibility of an excitation by upconversion. ‘The source was a Ti:sapphire laser. ‘The excitation power is conveyed to the sample by the same silica fiber with a coupling ratio of ~90%, and the emitted green fluorescence is transmitted by a second fiber, which captures only a small part of it, The hire laser power ranges from 150 mW to 1.5 W, de- pending on its emission wavelength (920 to 985 nm) and the argon-laser power level (9-12 W at 488 nm). Figure 3 gives the 550-nm green fluorescence yield (expressed as the ratio of the fluorescence signal to input power) versus the laser emission wavelength at. various pump levels for a BIZYT glass doped with 8% ytterbium and 2% erbium (molar concentration). As shown in this figure, the wavelength dependence of the efficiency is flat: the excitation wavelength can be between 960 and 980 nm without significant change in the upconversion response. This large tolerance is a noticeable advantage for future semiconductor laser excitation. Figure 4 illustrates the temperature behavior of the 520- and 550-nm fluorescent signals. As the tempera ture increases, the 550-nm signal continuously de- creases in amplitude, as expected since the ‘Syj2 level depopulates. “On the other hand, the 520-nm signal amplitude, which should show a steady increase with temperature (as measured when excited with an argon laser), goes to a maximum and then decreases, with the temperature tuming point being ~75°C. This behav- ior is attributed to the temperature dependence of the upconversion process.®! Nevertheless, the fluores- cence intensity ratio, showing a steady increase, does not reflect this last effect, as shown below. ‘This con- firms the assumption of the self-reference property of this transducing principle and its independence from the excitation mechanism. st experiment was done to demonstrate the ty of semiconductor laser excitation, which is a condition for the feasibility of the present approach. Semiconductor lasers emitting in the 970-980-nm range are not commercially available. However, such devices are under advanced development for erbium- doped fiber-optical amplifiers. ‘The experiment was carried out at the IBM Zarich Research Laboratory, Raschlikon, Switzerland, with their strained-layer ‘quaternary compound lasers delivering as much as 250 mW of de optical power in the desired wavelength region. ‘The samples were two BIZYT fluoride glass- Fig. 3. Optical response of a ytterbium-erbium codoped lass versus Ti:sapphire laser excitation wavelength jus argon-laser powers. Fig. 4. Erbium fluorescence signal amplitudes versus tem- perature obtained by upconversion with 970-nm semicon- ductor laser excitation.Fa ie 3102 OPTICS LETTERS / Vol. 15, No. 19 / October 1, 1990 Fig, 5. Quadratic correlation between the erbium fluores- ‘ent signals and the laser input squared power (the fluores. cent signals and laser power have been normalized to their maximum value). econ) Fig. 6. Intensity ratio of erbium fluorescent signals veraus temperature for a ZBLA fluoride optical fiber, codoped with ‘Me ytterbium and 2% erbium and excited by upconversion at 2 972-nm semiconductor laser wavelength. es, one doped with 9% ytterbium and 1% erbium and the other with 9.5% ytterbium and 0.5% erbium. ‘The expected quadratic dependence on the excita- tion power can be observed in Fig. 5, which represents the normalized fluorescence signal amplitudes versus the squared normalized input, power (1.0 corresponds to the maximum measured fluorescence signal, with 200 mW of power delivered by the semiconductor la- ser). ‘The quadratic dependence, similarly followed by the two fluorescent signals, is obeyed for laser pow- ers of up to ~130 mW, from where the dependence becomes somewhat linear, which reflects the theoreti- cal explanation advanced by Kingsley.'4 Finally, the upconversion fluorescent signal amplitudes are as high as those detected when the fluorescence results from direct absorption at 488 nm, showing that the overall yield is similar in both excitation processes at, equivalent power. For comparison, when a BIZYT gles singly doped with 39 erbium was excited by the ;pphire laser at 970 nm, the fluorescence signal at, 550'nm waa 30 dB lower than the seme signal in a codoped BIZYT glass (8% ytterbium and 2% erbium), demonstrating the energy-transfer efficiency. In conclusion, because of these results, we have de- signed and built a temperature measurement system. (including a 40-mW RCA laser emitting at 972 nm). Figure 6 gives the intensity-ratio temperature depen- dence for two sensor elements in preliminary tests of thissystem. ‘The result is similar to the one measured under argon absorption (see Fig. 2), which demon- strates the feasibility of reproducible temperature measurement by upconversion excitation of the "Hiii2 and 4Syipfluorescence lines of erbium in a fluoride host glass. This permits optical-fiber fluorescence tem- perature sensors to be operated with an IR semicon- ductor source of moderate power. ‘The authors are grateful to H. P. Weber and W. Lathy of the Applied Physics Institute, Bern Universi- ty, for making the Tisapphire laser available and for enlightened discussions and comments; to H. Jackel and A. Blacha of the Laser Science and Technology Department, IBM Zarich Research Laboratory, for permission to use their facilities and for making the semiconductor laser available; and to J. Lucas, Rennes University, for his help in the design of the fluoride glass and for making the samples. We thank E. Hae- fely & Co. Ltd., Bale, Rauscher & Stoekin, and Sissach and ABB Sécheron, Geneva, Switzerland, who sup- ported this study under Commission pour I'Encoura- gement A la Recherche Scientifique contract 1787-1. References 1, K.TT. V. Grattan, Meas, J. Int. Meas. Conf. 2, 134 (1984); G.D. Pitt, P. Extance, R. C. Neat, D.N. Batchelder, R E, Jones, J. A. Bamett, and R. H. Pratt, ISEE Proc. 1824, 214 (1986). 2. KT. V. Grattan, A. W, Palmer, and C. A. Wilson, J. Phys. E. 20, 1201 (1987). 3. AT. Agousti, K.T V. Grattan, and A, W. 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