Measurement Science and Technology Meas. Sci. Technol. 00 (2015) 000000 (8pp) UNCORRECTED PROOF Temperature sensing of micron scale polymer fibers using fiber Bragg gratings J Zhou1, Y Zhang1,2, M Mulle1 and G Lubineau1 1 King Abdullah University of Science and Technology (KAUST) Physical Sciences and Engineering Division, COHMAS Laboratory, Thuwal, 23955-6900, Saudi Arabia 2 Shanghai Jiao Tong University, School of Mechanical Engineering, State Key Laboratory of Mechanical Systems and Vibration, 800 Dongchuan Road, Minhang District, Shanghai 200240, People’s Republic of China E-mail: gilles.lubineau@kaust.edu.sa Received 18 February 2015, revised 8 April 2015 Accepted for publication 16 April 2015 Published Abstract Highly conductive polymer fibers are key components in the design of multifunctional textiles. Measuring the voltage/temperature relationships of these fibers is very challenging due to their very small diameters, making it impossible to rely on classical temperature sensing techniques. These fibers are also so fragile that they can not withstand any perturbation from external measurement systems. We propose here, a non-contact temperature measurement technique based on fiber Bragg gratings (FBGs). The heat exchange is carefully controlled between the probed fibers and the sensing FBG by promoting radiation and convective heat transfer rather than conduction, which is known to be poorly controlled. We demonstrate our technique on a highly conductive Poly(3,4-ethylenedioxythiophene)/poly(styrenesulfonate) (PEDOT/PSS)-based fiber. A non-phenomenological model of the sensing system based on meaningful physical parameters is validated towards experimental observations. The technique reliably measures the temperature of the polymer fibers when subjected to electrical loading. Keywords: fiber Bragg grating, conductive polymer, fiber, temperature, sensors AQ1 (Some figures may appear in colour only in the online journal) 1. Introduction these sensors do not provide good thermal contact with the probed surface. Their cooling surface may also be very large, which may induce significant measurement errors. RTDs and thermistors may be subjected to self-heating effects that may be detrimental if corrections are not made. These conventional electrical temperature sensors are reliable and accurate when they are fully surrounded by the environment they are supposed to sense. Although contact may be improved by using thermal conductive pastes, these sensors are more suitable for measurements of liquids and gases than for measurement of solids. In measuring the temperature of small objects, optical methods have been developed. This development stems from the progressive miniaturization of electronic components and the need to characterize their thermal behaviors. Optical methods have three major advantages: they do not require contact with the object, they provide a spatial distribution of the temperature measurements and they have a high spatial resolution. Using liquid crystal imaging, Aszodi et al During the last decade, significant developments in electrical conductive polymers have taken place [1–3]. Polymer fibers made of conductive polymers may be doped or de-doped with adequate solvents to tailor their conductive properties in such a way that they deliver significant joule effects when subjected to low current [4, 5]. These conductive polymer fibers can be used in wearable heating textiles as they are flexible and non-costly compared with carbon or metallic fibers [6]. Characterizing the thermal response of such heating fibers is important but remains very challenging because the small diameters (a few micrometers) of the fibers. The most prevalent technologies used to perform temperature measurements today are thermocouples, resistance temperature detectors (RTDs) and thermistors. Their size may be as small as a few tenths of microns and they allow high resolution measurements. However, with their typical bulbous ends, 0957-0233/15/000000+8$33.00 JNL:MST PIPS: 513253 1 TYPE: PAP TS: NEWGEN © 2015 IOP Publishing Ltd Printed in the UK DATE:30/4/15 EDITOR: IOP SPELLING: US J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 managed to obtain temperature maps with 5 μm separated isothermal lines [7]. Clayes et al used a thermo-reflectance method that allowed a lateral resolution of 1 μm [8]. Dohkkar et al demonstrated the capacity of a near-infrared thermography device to provide 1 μm resolution in both steady and transient states [9]. Infrared thermography is widely used in industry for thermal characterization, although due to the diffraction limit of infrared imaging, the spatial resolution is on the order of 5 μm. An alternative solution is to use optical fiber Bragg grating (FBG) devices. Such devices have been successful in thermal characterization under cryogenic conditions [10] or at very high temperature (up to 1000 °C) [11, 12]. FBGs have been embedded in composite materials to measure in-core temperatures during manufacturing processes [13, 14]. FBGs also have intrinsic advantages for sensing the temperature of small resistive polymer fibers subjected to current. They have a small size and a linear geometry; they are passive sensors and immune to electromagnetic interference. However, there is limited research on the use of FBGs to measure temperature on the micro-scale. An attempt was made by Antunes et al to measure the temperature of a copper wire [15]. The smallest tested wire had a diameter of 100 μm. The sensor was placed in contact along the wire and bonded with a thermal conductive compound to promote heat transfer. The acquired data was used in a model to predict the real temperature of the wires as a function of incident electrical current. This study included both conduction parameters and global radiation/ convection parameters that were identified by fitting a global single dimension equation. Because it was a very macroscopic model and the physical parameters were retrofitted to match the experimental results, it could not give reliable measures of the wire temperature. Motivated by the above considerations, we developed a new experimental approach and a related numerical model, in which we investigate the response of an FBG subjected to the joule effect produced by a 10 μm-diameter polymer fiber under current loading. This approach is guided by the idea that uncontrolled environmental parameters have to be minimized as much as possible. Direct contact between the polymer fiber and the FBG was avoided because the efficiency of the thermal transfer at the contact could not be determined with accuracy. We could partially solve this problem by using additional thermal paste but this solution would likely damage the polymer fiber and introduce a thermo-mechanical stress mismatch during heating. We therefore placed the FBG sensor as close as possible to the polymer fiber without contact and in the ambient air. Our model is based on a two-heat transfer mechanism: radiation and convection. The changes in temperatures can be detected at different voltages. We also run the measurement at different distances between the polymer fiber and the FBG sensor and investigate the dynamic thermal response. We then compared experimental results with the numerical model developed in COMSOL Multiphysics. Here we discuss the capability of the model to reproduce both the dependency of the measured temperature on voltage and the variation in the FBG temperature with respect to its distance to the heating source (the polymer fiber to be probed). These two observations are used to directly validate the model without tuning the model parameters. We finally discuss the validity of the overall approach to probing changes in the temperature of micro-sized and sensitive systems. 2. Experimental 2.1. Preparation of poly(3,4-ethylenedioxythiophene)/ poly(styrenesulfonate) (PEDOT/PSS) microfiber PEDOT/PSS microfibers were fabricated via wet-spinning as described in a previous study [5]. The fiber was wet-spun from a 22 mg mL−1 PEDOT/PSS dispersion (using a Clevios PH1000) followed by a vertical hot-drawing process. Wet fibers were pulled out from an acetone/isopropyl alcohol (acetone/IPA) coagulation bath. The resulting fibers had an average diameter of 10 μm and an electrical conductivity of 340 S cm−1. The fibers were prepared and fixed on a paper card to avoid fiber damage while handling the samples. 2.2. Preparation of FBG and calibration An FBG reflects a part of the incident light signal that is represented by a spectrum of wavelength [12, 13], it characterized by Bragg wavelength, λB, which corresponds to the spectrums peak. When the FBG is subjected to axial strain, ε, or temperature changes, ΔT, the peak shifts proportionally with these thermo-mechanical loadings. The Bragg wavelength variation can be expressed as [16, 17]: ΔλB = KTΔT + Kεε (1) λB where KT and Kε are related to the sensors sensitivities to temperature and strain, respectively. In this study the strain component was neglected as tests were carried out under stress-free conditions. The FBGs used here were 5 mm long and written on SMF28e standard fibers. The coating was removed along the FBG. The Bragg wavelength of the sensor was 1530 nm at room temperature. The temperature sensitivity (KT/λB) of the FBG was calibrated by immersing it together with a thermocouple in a beaker filled with water. The temperature of the water was increased gradually from 20 to 70 °C. The temperature and Bragg wavelength measurements were recorded at 1 Hz. The FBG sensitivity was determined to be 9.9 pm °C−1. 2.3. Experimental set-up and procedure The experimental set-up is shown in figure 1(a). The optical fiber and the polymer fiber were placed parallel to each other on a micro-manipulator, on the mobile and fixed part, respectively. The distance between the fibers could be controlled at a resolution of 5 μm. The micro-manipulator was placed inside a protective chamber to avoid environmental disturbances. Two conductive silver paste electrodes, spaced 20 mm apart, were connected to copper wires used to apply the electrical field. The effective length of the polymer fiber between 2 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 Figure 1. (a) Experimental setup for the temperature measurement of the polymer fiber using FBGs. (b) Microscope images of the optical fiber and the polymer fiber at different distances. Figure 2. (a) FBG spectra recorded at different voltages. The distance between the polymer fiber and the FBG is 100 μm. (b) Change of the wavelength versus voltage for different distances between the polymer fiber and the FBG. the two electrodes was 20 mm. To generate Joule heat on the polymer fibers, the electric field was applied to the fiber with a DC power supply (EXTECH instruments 382 280) and a pulse functional generator (Agilent Technology 81 150 A). The first instrument was used to investigate the thermal response under steady conditions and the second under cyclic conditions. The current flow in the fibers was monitored by using an U1252B digital multimeter. A Micron Optics sm125 unit was used for the acquisition of Bragg peak shifts and reflected spectra. The minimum distance between the polymer fiber and the optical fiber was set to 100 μm. It was then gradually increased to 6000 μm. The distance and the parallel placement between the fibers were controlled using a Leica DM2500 optical microscope. Images are shown in figure 1(b). For each distance, the voltage was applied to the polymer fiber with incremental steps of 2 V from 0 to 28 V. Electrical current data were captured at 1 Hz and FBG measurements at 2 Hz. The tests were conducted three times to evaluate repeatability and stability. In another series of tests, the dynamic thermal response of the polymer fiber was investigated at a distance of 100 μm. A cyclic square wave voltage was applied from 0 to 15 volt at frequencies of 0.02, 0.1, 0.25 and 0.5 Hz. 3. Experimental results and discussion 3.1. Raw measurement We first studied the raw data provided by the optical sensor. FBG spectra were recorded at each voltage step. Figure 2(a) presents these results for a distance of 100 μm between the polymer fiber and the FBG. The spectra from 0 to 28 V present a clear peak, indicating that the peak shits are reliably related to voltage change. Figure 2(b) shows changes in the Bragg peak wavelength for different distances between the polymer fiber and the FBG as a function of voltage steps. At the closest position (100 μm), the wavelength change from one voltage level to another is clearly pronounced. The sizes of wavelength steps reduced as the distance between the polymer fiber and the FBG increased. At 6000 μm, the FBG delivered a constant signal, indicating that at this distance the sensor was not able to detect any change. 3 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 Figure 3. (a) Temperature variation and current versus time for the polymer fiber placed 100 μm from the FBG. The voltage increased in steps of 4 volts from 0 to 28 V. (b) Changes in temperature versus voltage for increasing distances between the polymer and the FBG. Figure 4. (a) Dynamic thermal response of the polymer fiber at a distance of 100 μm from the FBG. A cyclic voltage was applied from 0 to 15 V at frequencies of 0.02, 0.1, 0.25 and 0.5 Hz. (b) The temperature and current changes with respect to time at 0.1 Hz. and the voltage affect the change in temperature as detected by the FBG. 3.2. Key experimental results In section 3.1, we presented raw measurements that were obtained for a certain voltage level and for a certain distance between the FBG and the polymer fiber. Here, we present the experimental observations to which the predictions of the numerical model presented in section 4 are compared. FBG data were transformed into temperature information according to equation (1). Curves of temperature variation to current are plotted with respect to time in figure 3(a). Results are given for the polymer fiber placed 100 μm from the FBG. Due to the current and the resistivity of the fiber, a joule effect was generated. This heat was transmitted by convection and radiation to the FBG. The temperature change (ΔT) detected by the optical sensor follows the current profile very closely. The maximum value of ΔT is 55.6 °C at 28 V. The response of the FBG to a voltage change took less than one second. Because heat is generated, transmitted and detected during this short delay, we can consider that this optical sensor is very sensitive. Figure 3(b) shows change in temperature as a function of voltage at different distances between the polymer fiber and the FBG. These results show how both the distance 3.3. Dynamic response We analyzed the dynamic response of the sensor/polymer fiber system by applying square wave voltage at different frequencies (figure 4(a)). The detected thermal response is stable and repeatable at each given frequency. From one frequency to another the temperature variation differs. The higher the frequency, the lower the temperature variation. This indicates that either joule heat is not generated to its maximum or that its transmission to the temperature sensor is not completed before another cycle takes place. Figure 4(b) presents details of temperature and current changes with respect to time at 0.1 Hz. The profile of the detected heat does not follow the square wave of the current. There is a small delay before reaching the steady state during both the heating and the cooling phase. The average delay is approximately 2.5 s. This represents the responsive limitation of the sensor/polymer fiber system under which the measured value will not be representative of the voltage input. 4 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 (a) Destination face m 20 m tion irec ep d Swe Source face variable distance (100 to 6000µm) y z x (b) Figure 5. (a) The geometry for the numerical model and the meshed polymer fiber and optical fiber. (b) The surfaces where boundary conditions are applied. 4. Modeling of the sensing set-up and it would be a totally arbitrary parameter to be identified by fitting experimental observations. This would make the model questionable from a physical point of view and we chose to eliminate the conduction mechanism by systematically making non-contact measurements. Two heat transfer mechanisms thus have to be included in the model: convection (which can still take place as all the experiments presented here were made in air) and radiation. Our model describes such exchanges between three elements: the polymer fiber, the FBG fiber and the environment. A major challenge in any sensing application is to resolve the physical quantity to be probed (here for example, the temperature of the polymer fiber or the heat flux it dissipates) as a function of the measured physical quantity (here, the temperature of the FBG). In other words, how can the physical quantities that are not directly measured by the sensor be evaluated if the FBG temperature is known? Answering this question requires a physically accurate model of the measurement system. This forward model can then be used to resolve the targeted physical quantity by solving the associated inverse problem. The first step is to model the heat transfer between the electrically loaded polymer fiber and the FBG. Among the three well-known heat transfer mechanisms (conduction, convection and radiation), conduction has been made impossible by avoiding contact in the experimental set-up. Indeed, modeling any conductive heat transfer that comes from direct contact between the polymer fiber and the FBG would be very challenging. Thermal conductivity of contacts is poorly defined 4.1. Model geometry, meshing and boundaries definitions The model geometry is shown in figure 5(a). The lengths of the polymer fiber (Ω1, diameter 10 μm) and the optical fiber including the 5 mm FBG (Ω2, diameter 125 μm) are both 20 mm. The distance between the surface of the polymer fiber and the surface of the FBG ranges from 100 to 6000 μm depending on the simulated experimental conditions. Quadrilateral elements are used for free meshing of the cross sections of both the FBG and polymer fibers. The plane 5 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 mesh is then extruded to create a three-dimensional mesh from this meshed cross section via a swept mesh method. We used 20 elements between the source and the destination faces. − + ∂Ωiz and ∂Ωiz are the start and end cross sections for the Ωi domain. ∂Ωil is the cylindrical surface of each domain (i = 1 or 2). ∂Ωi is the complete boundary for each domain (figure 5(b)). Table 1. Physical parameters selected for simulation of the electrical and thermal behaviors of the system. Property Symbol Unit Value σ1 k1 ε1 h1 S.m−1 W.m−1.K−1 — W.m−2.K−1 34000 0.22 0.9 85 k2 ε2 h2 W.m−1.K−1 — W.m−2.K−1 1.38 0.95 5 Polymer fiber Electrical conductivity Thermal conductivity Surface emissivity Convection coefficient 4.2. Formulation of the multiphysics problem FBG A coupled electrical/thermal problem is solved on the geometrical model described in figure 5 using the heat transfer and radiation capibilities of COMSOL Multiphysics. Electrical behavior. The start and end cross sections of the polymer fiber are subjected to ground and operating voltages (equations (2) and (3)). Flux conservation is assumed in the volume (equation (5)) and electrical insulation is assumed on the lateral surface (equation (6)). We assume a constant isotropic electrical conductivity, σ1 (equation (7)). Thermal conductivity Surface emissivity Convection coefficient − q ⋅ n = 0, ∀ M ∈ ∂Ωiz − ∪ ∂Ωiz +, i ∈ [1, 2] (12) •Thermal constitutive equations q = ki Φ, ∀ M ∈ Ωi, i ∈ [1, 2] (13) •Electrical potential equations: − V = 0, ∀ M ∈ ∂Ω1z (2) q con = hi(Troom − T ), ∀ M ∈ ∂Ωil , i ∈ [1, 2] (14) + V = Vmax, ∀ M ∈ ∂Ω1z (3) E = −∇V , ∀ M ∈ Ω1 (4) q rad = αi(Gim + Giam ) − εi(σSBT 4 ), ∀ M ∈ ∂Ωil , i ∈ [1, 2] (15) Thermal conductivity is isotropic (equation (13)). The convective exchange (qcon) is assumed to be, at every point of the lateral surfaces, ∂Ω1l and ∂Ωl2, proportional to the difference between the temperature and the temperature of the environment (Troom) (equation (14)). An important point is the choice of the convection coefficients. The convection coefficient of the FBG, h2, is set to the classical value for silica glass in air (table 1). For the polymer fiber, a higher value, h1, is selected because the water content in PEDOT/ PSS is relatively high and is progressively released during the heating process [5, 18]. This can then largely modify the moisture content in the vicinity of the surface of the polymer fiber, which classically yields to higher convection coefficients [19, 20]. The radiative flux, qrad, on each lateral surface is decribed by equation (15). In details: •Electrical equilibrium equations: ∇ ⋅ J = 0, ∀ M ∈ Ω1 (5) J ⋅ n = 0, ∀ M ∈ ∂Ω1l (6) •Electrical constitutive equations: J = σ1E , ∀ M ∈ Ω1 (7) Thermal behavior and thermal transfer. The polymer fiber and the FBG are both initially at room temperature (Troom) (equation (8)). The thermal flux, Φ, is classicially defined as the gradient of the temperature scalar function (equation (9)). A classical internal heat transfer equation is assumed (equation (10)). Qi is the internal heat source density (i = 1 or 2). The start and end cross sections are thermally insulated (equation (12)). The lateral surfaces of the polymer fiber, ∂Ω1l and of the FBG, ∂Ωl2, can exchange heat (equation (11)) by radiation (qrad) or by convection with their environment (qcon). •Each surface receives an inward flux, (Gim + Giam ), modulated by the absortivity of the continuum, αi. Gim is the mutual boundary-to-boundary irradiation. Giam is the irradiation received from the environment, which is assumed to behave as a black body. As such, Giam can be defined as: •Thermal potential equations T (t = 0, M ) = Troom, ∀ M∈Ω (8) 4 Giam = F amσSBTroom (16) Φ = −∇T , ∀ M∈Ω (9) where σSB is the Stefan–Boltzmann constant (σSB = 5.670 400 · 10−8 W.m−2.T−4). Fam is the ambient view factor whose value is equal to the fraction of the field of view that is not covered by other boundaries (0 ⩽ Fam ⩽ 1 must hold at all points). Fam is a geometrical quantity estimated by the finite-element package based on the model definition. •Thermal equilibrium equations ∂T ρi Ci = −∇ ⋅ q + Qi, ∀ M ∈ Ωi, i ∈ [1, 2] (10) ∂t − q ⋅ n = q rad + q con, ∀ M ∈ ∂Ωil , i ∈ [1, 2] (11) 6 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 Figure 6. (a) Experimental and modeling results of different distances at 28 V. (b) Experimental and modeling results of different voltages at a distance of 100 μm. •Each surface loses an outward flux, (σSBT4), assuming the Stefan–Boltzmann law, which is modulated by the emissivity of the continuum, εi. Figure 6(a) compares the experimental and modeling results at different distances from 100 to 6000 μm with a fixed applied voltage of 28 V. Figure 6(b) compares experimental and modeling results at different voltages from 0 V to 28 V with a fixed distance of 100 μm. We observe that the experimental measurements and more importantly, their changes with distance and voltage, are well predicted by the model without introducing numerous phenomenological parameters. The fact that the change with distance is well predicted demonstrates that the introduced heat transfer mechanisms are correct and that the model can reliably reconstruct quantities of interest that are useful for design purposes. To simplify the process, each continuum (either the polymer fiber or the optical fiber) is assumed to behave as a grey body with equal absortivity and emissivity (αi = εi) [21, 22]. Heat source. The coupling between the electrical and thermal behaviors is generated by the Joule effect that produces the body heat source in the polymer fiber. As such, Q1 is defined by equation (17). Of course, no heat source is assumed in the FBG so that Q2 is taken to be equal to zero. Q1 = E ⋅ J , ∀ M ∈ Ω1 (17) Both transient and steady-state models have been developped. Because the stabilization of the measured temperature is very quick (figure 3), we prefer to rely only on the steady-state measurements. Then, the above set of equations can be simplified by assuming it is independent of time. A stationary solver is ( ∂T used by assuming that terms ρi Ci ∂t 5. Conclusion Temperature measurements have been conducted at the micron scale to probe changes in temperature of conductive polymer fibers when electrically loaded. Such fragile fibers can be probed only by non-contact measurement systems. The ability and efficiency of FBGs to supply such measurement has been demonstrated in this framework. This is a step toward better understanding of the response of such fibers and their use in heating devices. A key point is that unreliable heat transfer mechanisms have been carefully removed. It was possible to simulate the whole sensing configuration without extensive calibration or assumptions in the modeling part. We demonstrated that a model directly based on both radiation and conduction that utilizes the classical material parameters that characterize involved materials provides very pertinent results. This model can now be used to extract, depending on the information needed for each application, any quantity of interest that is not directly measured in the experiments such as the temperature of the polymer fiber, the heat flux dissipated by the polymer fiber and the relative fractions of the radiated and convective heat flux. Future work will focus on the optimization of such conducting fibers that is possible thanks to the accuracy of this measurement technique. )) in equation (10) vanish. This choice leads to a more robust model as it reduces the number of material parameters to be identified (knowing that any mistake in the material parameters introduces errors in the reconstruction of the measured temperature of the polymer fiber). A transient model would also need to characterize the heat capacity, Ci and the density, ρi, for both domains Ω1 and Ω2. These parameters are not needed when solving the steadystate equations. All physical parameters used for the simulation are listed in table 1. These are either very classical values for glass or have been identified in previous publications about conductive fibers [5]. 4.3. Modeling results and comparison with experiments The experimental results presented in figures 2 and 3 are simulated by varying the applied voltage from 0 to 28 V and the distance, l, between the polymer fiber and the FBG from 100 to 6000 μm. 7 J Zhou et al Meas. Sci. Technol. 00 (2015) 000000 Acknowledgments AQ2 intensified CCD camera and frame integration Meas. Sci. Technol. 18 2696–703 [10] Lupi C, Felli F, Ippoliti L, Caponero M A, Ciotti M, Nardelli V and Paolozzi A 2005 Metal coating for enhancing the sensitivity of fibre Bragg grating sensors at cryogenic temperature Smart Mater. 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