Home Search Collections Journals About Contact us My IOPscience A method for evaluation of the inhomogeneity of thermoelements This content has been downloaded from IOPscience. Please scroll down to see the full text. 2009 Meas. Sci. Technol. 20 055102 (http://iopscience.iop.org/0957-0233/20/5/055102) View the table of contents for this issue, or go to the journal homepage for more Download details: IP Address: 132.174.254.159 This content was downloaded on 28/05/2015 at 02:56 Please note that terms and conditions apply. IOP PUBLISHING MEASUREMENT SCIENCE AND TECHNOLOGY Meas. Sci. Technol. 20 (2009) 055102 (9pp) doi:10.1088/0957-0233/20/5/055102 A method for evaluation of the inhomogeneity of thermoelements Y A Abdelaziz1 and F Edler2 1 2 National Institute for Standards, Tersa St, Elharam, 12211 Giza, Egypt Physikalisch-Technische Bundesanstalt, Abbestraße 2-12, 10587 Berlin, Germany E-mail: [email protected] and [email protected] Received 12 December 2008, in final form 11 February 2009 Published 27 March 2009 Online at stacks.iop.org/MST/20/055102 Abstract Thermoelectric inhomogeneity is the spatial variation of the Seebeck coefficient along a thermoelement. It is often considered to be the largest contribution of an uncertainty budget in thermocouple calibration. In this work, investigations of inhomogeneities were performed on single thermoelements, using a heater with short movable heating zones (two-gradient method). We chose platinum wires which are commonly used in noble metal thermocouples and copper wires which are available in good homogeneity and which are commonly used in base metal thermocouples. The results of different investigations of the thermoelements are presented. Keywords: thermoelements, thermoelectric inhomogeneity, Seebeck coefficient. In addition to the temperature difference, the measured emf is caused by the Seebeck effect only, and therefore, the Seebeck inhomogeneity is of practical interest in thermometry. The Seebeck inhomogeneity is defined in [1] by equation (2): 1. Introduction Thermocouples are the most widely used electrical sensors in temperature measurements. They are characterized by a simple construction. Two dissimilar wires electrically insulated are joined at one end. A temperature difference between this common junction (measuring junction) and the open end (reference junction) causes a potential difference which can be measured between the two dissimilar wires at their open ends. This thermoelectric voltage is called electromotive force (emf) and occurs in any conductor which is located in a nonuniform temperature region. It can be described by equation (1): dE = S(T ) · dT , δS(T , x) = S(T , x) − SN (T ), expressing the abnormal spatial variation of the Seebeck coefficient along a thermoelement relative to a normal reference function, SN (T ). Inhomogeneity effects are measured by exposing the thermocouple or a single thermoelement to defined temperature gradients. Different methods can be applied. The common method to investigate assembled thermocouples is to submerge them slowly into a fixed-point cell during melting or freezing or into a liquid bath maintaining the temperatures of the measuring and reference junction constant while monitoring the output emf. Thus, any deviation of the measured emf is an indication of inhomogeneities. Another method, the two-gradient method, can also be used to investigate single thermoelements before they are assembled. Most of the previous researches studied thermocouple inhomogeneity at assembled thermocouples [2–8]. In this work, the inhomogeneity tests were performed on single thermoelements using short movable heating zones with two temperature gradients. (1) where dE is the differential voltage generated by sections of the wires in a temperature gradient, S(T ) is the Seebeck coefficient and T is the temperature. As long as the Seebeck coefficient, S(T ), is a function of only temperature and not of the position x along the wires, dE depends on the end temperatures only. Such wires are said to be homogeneous. Often most of the thermoelements used are inhomogeneous because of thermal and mechanical stresses and environmental influences. This results in localized changes in the Seebeck coefficient and can be considered as the most important uncertainty contribution in measuring temperatures by using thermocouples. 0957-0233/09/055102+09$30.00 (2) 1 © 2009 IOP Publishing Ltd Printed in the UK Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler unchanged. The left-hand side of the heater completely covers an inhomogeneous section and the right-hand side covers only this inhomogeneous section between 217 ◦ C and TC (about 200 ◦ C). Therefore, the output emf remains constant. 2. Two-gradient method The two-gradient method in which a movable heater is used is a simple and precise method to assess qualitatively and quantitatively inhomogeneities in thermoelements. A movable heater or furnace with known temperature gradients is moved along the thermoelement (or thermocouple) under investigation with a known and uniform velocity. In this way the thermoelement is exposed to two temperature gradients, one on each side of the heated zone. Both temperature gradients are reversed left to right. Therefore, the two emfs generated at the positions of the gradients will be of opposite sign but of the same magnitude as long as there are no inhomogeneities in the thermoelement. In this case, the resulting emf measured at the two ends of the thermoelement will be zero. On the other hand, a spatial variation of the Seebeck coefficient caused by inhomogeneities will result in an emf that deviates from zero if such inhomogeneous sections of the thermoelement are exposed to the temperature gradients. This emf measured using the two-gradient method will not directly give a quantitative indication of the inhomogeneity as obtained using a one-gradient measurement. With the twogradient method, the resulting emf as a function of the position of the heating zone is actually a measure of the derivative of the corresponding emf measured by using the onegradient method [9]. Because of the compensating effect of the two oppositely directed temperature gradients, a direct reading of the emf differences would result in a quantitative underestimation of inhomogeneity-caused uncertainties. Figure 1 shows a model of scanning a thermoelement by using a movable heater (top) and a corresponding experimental scanning curve of a copper wire (bottom). In this case, the maximum temperature of the heater is higher than a critical temperature TC , at which inhomogeneities will be induced. Part (a) of figure 1 shows the output emf at different positions of the heater. Part (b) shows the thermoelement containing a homogeneous section ‘white’, an inhomogeneous section induced by the movable heater ‘black’ and a third section which becomes inhomogeneous by the movable heater during scanning. The temperature profiles of the movable heater at different positions (1, 2, 3 and 4) are shown in part (c) of figure 1. The resultant emf can be described as follows. 3. Experimental set-up Figure 2 shows the schematic diagram of the experimental set-up. Both ends of the investigated thermoelement were maintained at the same temperature in an electrically shielded box. Therefore, any deviation of the measured emf from zero is an indication of inhomogeneity when the short, welldefined heating zone is moved along the wire. The heater was moved with a constant velocity of 2 mm min−1 . The measured emfs using a nanovoltmeter Keithley model 2182 were recorded, displayed and stored automatically using a R program. The measurement uncertainty of the LabVIEW emfs was estimated to a value of about ±0.1 μV, mainly caused by the short-time stability of the nanovoltmeter during the scans. The stability of the heater temperature can be neglected because of the applied two-gradient method (difference measurement). Environmental influences were minimized by using the shielded terminal box and would influence both junctions equally. Therefore, almost no parasitic emfs have to be considered. The temperature profiles of the movable heater used to perform the inhomogeneity tests were measured using a sheathed type J thermocouple. The thermocouple was inserted into an alumina tube and maintained at a fixed position. A second sheathed thermocouple identical to it in geometry was inserted into the alumina tube from the other side to adjust a symmetrical condition concerning heat flux effects along the alumina tube during the measurement of the temperature profiles. The heater was moved along the type J thermocouple. For example, two different temperature profiles, but of the same maximum temperature (about 227 ◦ C), are shown in figure 3. The profile with the wider heating zone was achieved by inserting a small aluminum tube into the heater coil. The width of the heater is dg . 4. Investigation of a copper wire Position 1. The inhomogeneous part of the thermoelement induced by the heater itself is exposed to two symmetrical temperature gradients on both sides of the movable heater. The output emf is zero because the temperature gradients generate two emfs of the same amount but of opposite signs. A pure copper wire (99.999% purity, 0.5 mm diameter) of high homogeneity was investigated. It was cleaned using pure ethanol and distilled water to remove the layer of brown-black copper oxide and surface traces. For the scanning process, the copper wire was connected to the voltmeter directly. So, the resulting emf of the nearly homogenous wire should be zero and any deviation would indicate inhomogeneities, when the gradients of the heating zone pass inhomogeneous sections of the wire. In the next step, a well-directed inhomogeneity induced in the copper wire was used to study and to quantify local inhomogeneity effects. For this purpose, a small segment of the copper wire was exposed briefly to a temperature of about 350 ◦ C. In figure 4, the scanning results at 200 ◦ C before and after inducing this inhomogeneity are presented. The small emf changes along the copper wire before inducing the inhomogeneity are within about ±0.1 μV, which indicates its Positions 1 to 2. During the movement of the heater from positions 1 to 2, the left-hand side of the temperature profile of the movable heater covers an increasing range of the inhomogeneous section of the thermoelement, but the right-hand side covers only the inhomogeneous section of the thermoelement which becomes inhomogeneous during scanning, and it is exposed to a temperature higher than the critical temperature TC . Therefore, during scanning the output emf increases uniformly until the heater reaches position 2. Positions 2 to 3 and 4. A further movement of the heater does not change the output emf because the geometrical condition is 2 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 0.5 0.4 emf, μV 0.3 0.2 0.1 0 -0.1 -0.2 0 50 100 150 200 250 300 distance, mm Figure 1. Scanning of a thermoelement using a movable heater. Figure 2. Schematic diagram of the experimental set-up. of the maximum of the inhomogeneity which corresponds to the contact point of the copper wire with hot temperature. Furthermore, the difference between the two emf curves along the whole scanned length of the copper wire indicates that not only a small localized inhomogeneity in the middle of the copper wire was induced by the temperature of 350 ◦ C but also extended parts of the thermoelement were influenced, which resulted in abnormal variations of the Seebeck coefficient over good homogeneity. The constant deviation of the measured emf from zero (1.0–1.2 μV) was caused by the offset emf of the voltmeter. The measured emfs of the manipulated wire differ completely from that of the homogeneous one. A symmetrical sine waveform was measured, with maximum and minimum deviations from the original emf curve of about ±0.7 μV. The intersection point between both the measurements before and after introducing the inhomogeneity indicates the position 3 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 14000 small heating zone wide heating zone 12000 emf, μV 10000 8000 6000 4000 2000 0 0 20 40 60 80 100 distance, mm 120 140 160 180 Figure 3. Temperature profiles of the movable heater at about 227 ◦ C. 2 before inducing inhomogeneity 1.8 after inducing inhomogeneity 1.6 emf, μV 1.4 1.2 1 0.8 0.6 0.4 0.2 0 0 20 40 60 80 100 distance, mm 120 140 160 180 Figure 4. Inhomogeneity scan at 200 ◦ C of the pure copper wire before and after inducing inhomogeneity. 12000 10000 emf, μV 8000 6000 4000 2000 0 0 1 2 3 4 5 6 7 8 distance, mm 9 10 11 12 13 14 Figure 5. Temperature profile of the movable heater at 200 ◦ C. way, the compensation effect of the two oppositely directed temperature gradients is considered. In general, at the position xm of the heater, the measured emf corresponds to the emf difference between positions x1 and x2 (figure 5). If the emf at position x1 is known, the emf of position x2 can be a range between 40 mm and 160 mm of the wire. Figure 5 shows the corresponding temperature profile of the movable heater at 200 ◦ C. For the quantitative estimation of the copper wire inhomogeneity, the method proposed in [9] was used. In this 4 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 1.8 measured data calculated data 1.6 emf, μV 1.4 1.2 1 0.8 0.6 0.4 0 20 40 60 80 100 120 140 160 180 distance, mm Figure 6. Comparison of the measured and calculated emfs of the homogeneous copper wire. 2.8 measured data calculated data 2.4 emf, μV 2 1.6 1.2 0.8 0.4 0 0 20 40 60 80 100 120 140 160 180 distance, mm Figure 7. Measured and calculated emfs of the copper wire containing the induced inhomogeneity at 200 ◦ C. maximum emf difference of about 1.4 μV obtained from the directly measured emf curve. calculated easily. If we assume that the first part of the thermoelement is homogeneous (see figure 4), the starting emf for the calculation at x1 is zero. The distance dg between the two temperature gradients must be known. For applying this method, the incremental steps to calculate the absolute emf at each position were 1 mm. Figure 6 shows the measured and the calculated emfs of the nearly homogenous copper wire at a heater temperature of 200 ◦ C, before the inhomogeneity was induced. The calculated emfs were corrected by the offset emf of 1.1 μV. The measured and the calculated emfs of the copper wire containing the induced inhomogeneity are shown in figure 7. Both emf curves can be used as a qualitative evaluation of the inhomogeneity but the calculated emf curve can also be used as a quantitative estimation of the inhomogeneity. The peak of the calculated curve at the position of about 90 mm from the starting point of scanning corresponds to the inflection point of the measured emf curve which indicates the position of the induced inhomogeneity. The maximum emf difference of the calculated curve as a measure of the inhomogeneity amounts to about 1.8 μV, which is by about 0.4 μV higher than the 5. Investigation of a platinum wire A new platinum wire was heated electrically at 1300 ◦ C for 5 h, and then assembled in a capillary tube and annealed in a horizontal furnace at 1100 ◦ C for about 4 h to reach a homogeneous state. Figure 8 shows the measured emf curves of the Pt wire using the movable heater with different temperature profiles (figure 3) at about 227 ◦ C. The measured emf curves offer deviations from a constant emf value indicating the presence of inhomogeneities in the platinum wires in the order of about ±0.25 μV (heater with small zone) and of about ±0.4 μV (heater with wide zone). These differences indicate the influence of different heater profiles which have to be considered for the quantitative estimation of inhomogeneities by applying the method proposed in [9]. The lower emf changes using the heater with a smaller heating zone are a result of the more distinctive compensating effect caused by the two narrower temperature gradients of the heater. 5 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 0.6 wide heating zone small heating zone 0.4 0.2 emf, μV 0 -0.2 -0.4 -0.6 -0.8 -1 0 100 200 300 distance, mm 400 500 600 Figure 8. Scanned platinum wire using the movable heater with wide and small heating zones before inducing an inhomogeneity at 227 ◦ C. 0.3 before inducing inhomogeneity after inducing inhomogeneity 0.2 0.1 emf, μV 0 -0.1 -0.2 -0.3 -0.4 -0.5 0 100 200 300 distance, mm 400 500 600 Figure 9. Scanned platinum wire using the movable heater with the small heating zone at 227 ◦ C before and after inducing inhomogeneity. 0.6 before inducing inhomogeneity after inducing inhomogeneity 0.4 0.2 emf, μV 0 -0.2 -0.4 -0.6 -0.8 -1 0 100 200 300 distance, mm 400 500 600 Figure 10. Scanned platinum wire using the movable heater with the wide heating zone at 227 ◦ C before and after inducing inhomogeneity. In the next step, an extra inhomogeneity was induced in the platinum wire by cutting it at a distance of about 290 mm from the starting point of scanning, and welding both ends together. Figures 9 and 10 show the scanning results of the platinum 6 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 0.6 wide heating zone small heating zone 0.4 0.2 emf, μV 0 -0.2 -0.4 -0.6 -0.8 -1 0 100 200 300 distance, mm 400 500 600 Figure 11. Scanned platinum wire using the movable heater with wide and small heating zones after inducing inhomogeneity at 227 ◦ C. 0.8 measured data calculated data 0.6 emf, μV 0.4 0.2 0 -0.2 -0.4 -0.6 0 100 200 300 distance, mm 400 500 600 Figure 12. Measured and calculated data of the scanned platinum wire at 227 ◦ C using the movable heater with the small zone. one [9] by using the small heating zone. The same position of the inhomogeneity (peak in the recalculated curve, inflection point in the measured curve) was found at about 290 mm from the starting point of the scanning. Also in figure 13, the position of the inhomogeneity in both curves is the same. Furthermore, comparing figures 12 and 13, independent of the different geometries of the temperature profiles, the same position of the inhomogeneity could be found. Simultaneously, the maximum emf differences in both calculated emf curves were found to have about the same value of (1.0 ± 0.1) μV. It should be mentioned that the maximum emf differences in the directly measured curves differ from each other considerably, 0.6 μV and 1.0 μV for the heater with the small and wide zones, respectively. The results of several scanning runs of the inhomogeneous platinum wire at 227 ◦ C and 410 ◦ C (two runs at each temperature) are presented in figures 14(a) and (b) to prove the reproducibility of the homogeneity tests. Here, the movable heater with a small heating zone was used. Figure 14(a) shows the measured emfs and figure 14(b) shows the calculated data according to Holmsten. wire before and after inducing the defined inhomogeneity by using the movable heater with a small heating zone (figure 9) and the one with a wide heating zone (figure 10) at about 227 ◦ C. A large additional emf having a sine waveform was observed at the position of the induced inhomogeneity (about 290 mm from the starting point). Figure 11 compares the measured emf curves of the inhomogeneous platinum wire by using two different heater profiles (small and wide heating zones) at a temperature of 227 ◦ C. In both cases, the intersection of the emf curves with the x-axis (offset of about −0.2 μV) clearly indicates the position of the localized inhomogeneity at about 290 mm from the starting point. The maximum emf difference found using the small heating zone was about 0.6 μV; the maximum emf difference found using the wider heating zone amounts to about 1.0 μV. This is, considered relatively, the same value of the difference found in the former ‘homogeneous’ platinum wire (figure 8) by using the two different heating zones. The results of the qualitative assessment and the quantitative estimation of the induced inhomogeneity of the platinum wire are presented in figures 12 and 13. Figure 12 shows the measured emf curve compared with the recalculated 7 Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler 0.8 measured data calculated data 0.6 0.4 emf, μV 0.2 0 -0.2 -0.4 -0.6 -0.8 -1 0 100 200 300 distance, mm 400 500 600 Figure 13. Measured and calculated data of the scanned platinum wire at 227 ◦ C using the movable heater with the wide zone. 1 at at at at emf, μV 0.5 227°C 227°C 410°C 410°C 0 -0.5 -1 -1.5 0 100 200 300 400 500 600 distance, mm (a) 2 at at at at 1.5 227°C 227°C 410°C 410°C emf, μV 1 0.5 0 -0.5 -1 -1.5 0 100 200 300 distance, mm 400 500 600 (b) Figure 14. Reproducibility of the homogeneity tests for measured and calculated data of the scanned platinum wire at different temperatures. (This figure is in colour only in the electronic version) The temperature difference T in column 4 is the difference between the heater temperature and the room temperature which was constant at 23 ◦ C during the measurements. The abnormal variations of the Seebeck coefficient were calculated according to equation (3): The results of the quantitative estimation of the induced inhomogeneity of the platinum wire at different temperatures (227 ◦ C, 303 ◦ C and 410 ◦ C, small heating zone) using the same method of calculation [9] as was described previously are given in table 1. The absolute Seebeck coefficients of platinum at different heater temperatures are listed in column 2 [10]. δS(P t) = emf/T . 8 (3) Meas. Sci. Technol. 20 (2009) 055102 Y A Abdelaziz and F Edler Table 1. Quantitative estimation of the induced inhomogeneity of the platinum wire at different temperatures. Temperature of heater TH (◦ C) 227 303 410 SN (Pt) at TH (μV K−1 ) −9.53 −10.83 −12.46 Maximum emf difference (μV) T (K) δS(Pt) (μV K−1 ) δS(Pt)/SN (Pt) 0.9 1.3 2.2 204 280 387 4.41 × 10−3 4.64 × 10−3 5.68 × 10−3 4.63 × 10−4 4.29 × 10−4 4.56 × 10−4 The nearly constant ratio of the abnormal Seebeck coefficient and the absolute Seebeck coefficient of platinum of about 4.5 × 10−4 at different temperatures confirms the correlation found in [4] that the inhomogeneity measured at one temperature can be expressed as a percentage of the total emf at this temperature. A similar expression f = S/S, a so-called inhomogeneity factor, was introduced in [5] for characterizing thermoelements. References [1] Reed R P 1992 Thermoelectric inhomogeneity testing: Part I. Principles Temperature: Its Measurement and Control in Science and Industry vol 6 ed J F Schooley (New York: American Institute of Physics) pp 519–24 [2] Bentley R E 2000 A thermoelectric scanning facility for the study of elemental thermocouples Meas. Sci. Technol. 11 538–46 [3] Jonathan V P 2007 Quantitative determination of the uncertainty arising from the inhomogeneity of thermocouples Meas. Sci. Technol. 18 3489–95 [4] Jahan F and Ballico M 2003 A study of the temperature dependence of inhomogeneity in platinum-based thermocouples Temperature: Its Measurement and Control in Science and Industry (Chicago, IL, 2002) (AIP Conf. Proc.) pp 469–74 [5] Kim Y-G, Gam K S and Lee J H 1997 The thermoelectric inhomogeneity of palladium wires Meas. Sci. Technol. 8 317–21 [6] Kim Y-G, Gam K S and Kang K H 1998 Thermoelectric properties of the Au/Pt thermocouple Rev. Sci. Instrum. 69 3577–82 [7] Reed R P 1992 Thermoelectric inhomogeneity testing: Part II. Advanced methods Temperature: Its Measurement and Control in Science and Industry vol 6 ed J F Schooley (New York: American Institute of Physics) pp 525–30 [8] Zvizdic D and Veliki T 2006 Testing of thermocouples for inhomogeneity XVIII Imeko World Congress: Metrology for a Sustainable Development (Brazil) [9] Holmsten M, Ivarsson J, Falk R, Lidbeck M and Josefson L-E 2007 Inhomogeneity measurements of long thermocouples using a short movable heating zone Int. J. Thermophys. 29 915–25 [10] Roberts R B 1981 The absolute scale of thermoelectricity II Phil. Mag. B 43 1125–35 6. Summary Two thermoelements (a copper wire and a platinum wire) were investigated for inhomogeneity by using a movable heater with two symmetrical temperature gradients. In the case of the copper wire the investigation technique was demonstrated. The main benefit of the two-gradient method is the simple local verification of inhomogeneities in thermoelements, independent of the shape and magnitude of the heating zone. The quantitative estimation of inhomogeneities concerning their influence on the uncertainty of a temperature measurement requires a numerical recalculation of the directly measured emf curve, which is a measure of the derivative of the corresponding emf measured by using the one-gradient method. It was found that the magnitude of the directly measured emf depends on the temperature and on the shape of the heating zone, i.e. on the temperature gradients T and on the width dg of the zone. Applying the method of Holmsten [9], the recalculated emf was found to be independent of the shape of the heating zone but proportional to its temperature, i.e. directly proportional to the value of the Seebeck coefficient of the thermoelement. 9