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Apparatus for the High Temperature Measurement of the Seebeck Coefficient in Thermoelectric Materials

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Apparatus for the High Temperature Measurement of the Seebeck Coefficient in Thermoelectric Materials REVIEW OF SCIENTIFIC INSTRUMENTS 83,065101(2012) Apparatus for the high temperature measurement of the Seebeck coefficient in thermoelectric materials Joshua Martina) Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899, USA (Received 24 February 2012; accepted 15 May 2012; published online 1 June 2012) The Seebeck coefficient is a physical parameter routinely measured to identify the potential thermo- electric performance of a material. However, researchers employ a variety of techniques, conditions, and probe arrangements to measure the Seebeck coefficient, resulting in conflicting materials data. To compare and evaluate these methodologies, and to identify optimal Seebeck coefficient measurement protocols, we have developed an improved experimental apparatus to measure the Seebeck coefficient under multiple conditions and probe arrangements (300 K–1200 K). This paper will describe in detail the apparatus design and instrumentation, including a discussion of its capabilities and accuracy as measured through representative diagnostics. In addition, this paper will emphasize the techniques required to effectively manage uncertainty in high temperature Seebeck coefficient measurements. [http://dx.doi.org/10.1063/1.4723872] I. INTRODUCTION The continued development of higher efficiency TE ma- terials requires thorough characterization of the electrical The Seebeck effect is a thermoelectric (TE) phenomenon and thermal transport properties. Due to its intrinsic sensi- that enables the conversion of an applied thermal gradient into tivity to the electronic structure, the Seebeck coefficient is an electric potential. This effect can be quantified through a one physical parameter that is routinely measured to identify constant of proportionality termed the Seebeck coefficient, amaterial’spotentialthermoelectricperformance.However, S !V /!T, under the assumptions in the differential ab ab researchers employ a variety of techniques, conditions, and technique,= 1 where !V is the electric potential between two ab probe arrangements to measure the Seebeck coefficient,1, 10–14 different materials a and b, and !T T T is the applied 2 1 resulting in conflicting materials data and further compli- temperature difference.1–7 According= to this− definition, the cating the confirmation of reported higher efficiency ther- measured Seebeck coefficient S requires the correction S ab ab moelectric materials. In an effort to compare and evaluate S S ,whereS is the contribution of the second conduc- b a b these methodologies, and to identify optimal Seebeck coeffi- tor,= to− obtain S ,theSeebeckcoefficientofthesample(here- a cient measurement protocols, we have developed an improved after referred to as S). In n-type (p-type) semiconductors, the experimental apparatus15 to measure the Seebeck coefficient electric potential establishes in the opposite direction (same under multiple conditions and probe arrangements, and the direction) of the thermal gradient resulting in a negative (pos- electrical resistivity at high temperature (300 K–1200 K). itive) Seebeck coefficient. This convention ensures agreement Electrical resistivity measurements will be presented sepa- between the Seebeck coefficient and the sign of the carriers. rately in a forthcoming publication. This paper will include a However, measurements of n (carrier concentration) and R H general overview of thermoelectric metrology, the apparatus (Hall coefficient) are often required to fully evaluate the elec- design and instrumentation, and a discussion of its capabili- tronic structure,8, 9 as the Seebeck coefficient is not explicitly ties and representative diagnostics. We will further emphasize indicative of the majority carrier. the techniques required to effectively manage uncertainty in Materials that exhibit large absolute Seebeck coefficients high temperature Seebeck coefficient measurements. (S 100 µV/K–200 µV/K at their target operation tempera- ture),≈ in addition to other optimal physical properties, are con- sidered candidates for use in thermoelectric applications.3–7 II. SEEBECK COEFFICIENT METROLOGY These applications include automotive engine waste heat recovery, power generation, spot cooling, and solid-state re- Measurement of the relative Seebeck coefficient, espe- frigeration. The dimensionless figure of merit, ZT S2σ T/κ, cially at high temperature, requires a minimum of three volt- = defines the effectiveness of a TE material, where σ is the elec- age measurements: one for the thermoelectric voltage !V trical conductivity, T the absolute temperature, and κ the total and one each for the hot and cold thermocouple voltage for thermal conductivity. However, optimizing these interdepen- T2 and T1,respectively,thatdeterminethetemperaturedif- dent physical parameters to achieve commercially practical ference !T. Acquisition protocols for these parameters must efficiencies is challenging, requiring a tailored combination adhere to the following criteria, defined previously1 as 1. the of properties not readily available in nature. measurement of the voltage and temperature at the same loca- tions and at the same time; 2. probe interfaces with the sample that are Ohmic and isothermal; and 3. the acquisition of small a)E-mail: [email protected]. Fax: 301-975-5334. voltages with minimal extraneous contributions. Under these 0034-6748/2012/83(6)/065101/9/$30.00 83,065101-1 This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP: 129.6.180.135 On: Thu, 26 Jun 2014 20:12:20 065101-2 Joshua Martin Rev. Sci. Instrum. 83,065101(2012) conditions, the electric potential emergent under an applied thermal gradient is given by1 T2 Vab(T1, T2) Sab(T)dT = !T1 T2 [Sb(T) Sa(T)]dT, (1) = − !T1 where Sa(T) is the absolute Seebeck coefficient of the sample being measured and Sb(T) is the known Seebeck coefficient of the reference wires. It is assumed that materials a and b are chemically and physically homogeneous and isotropic, such that Vab is explicitly a function of (T1,T2)andisindependent of the temperature distribution between the interfaces.16 Historically, there exist two primary probe arrangements. In the axial-flow arrangement (2-probe), the temperature dif- ference and the electric potential are measured on the probes which are in direct contact with the ends of the specimen (Figure 4). This is the arrangement preferred by Goldsmid and Tritt12 for improved thermal and electrical contact. However, FIG. 1. (a) Photograph of the instrumentation cabinet for the high tempera- ture thermoelectric apparatus. (b) Photograph of the sample probe. (c) Photo- many Seebeck coefficient apparatus also concurrently mea- graph of an individual probe arm without the heater coil detailing the machin- sure resistivity, requiring additional voltage contacts away ing of the tungsten component. (d) Four-probe thermocouple spring mounts. from the ends of the sample. In the potentiometric arrange- ment (or 4-probe), the temperature difference and the voltage difference are measured at two points on the sample (or in- each mounted at the focal point of a parabolic gold reflec- serted within the sample) equidistant from the hot and cold tor. This geometry provides axial and radial thermal profiles sinks and on the axis parallel to the thermal gradient. To main- that are temporally and spatially consistent. The temperature tain accuracy, the diameter of each temperature/voltage probe is tuned via a Eurotherm 7100A power controller and a Eu- must be much smaller than the effective distance between rotherm 3508 temperature controller. Since the emitted IR fre- them. quencies are dependent on the voltage supplied, the power There is little comparative evidence to substantiate which controller is placed between a 144 V output centertap trans- arrangement provides the most accurate determination of tem- former and the IR furnace, and is further equipped with an perature and voltage difference at the same points. We have auxiliary power supply that is in phase with the transformer therefore developed an apparatus capable of in situ compari- input voltage. Infrared elements typically operate under phase 17 son. An apparatus developed by Bowers in 1959 averaged angle firing modes which can result in the generation of sig- the results obtained by both of these arrangements. The See- nificant radio frequency interference with the voltage mea- beck coefficients were consistent within 10% up to 800 ◦C. surement instrument. Therefore, the selected power controller However, there was no estimation made of the overall mea- operates under advanced single cycle firing. In this mode, the surement uncertainty, so this result may be regarded as pre- power is only active between multiples of zero-voltage cross- 18 liminary. Wood also compared the results of thermocouples ings that track the input line frequency, effectively eliminating pressed on the ends of a sample with those obtained by insert- radio frequency noise. The furnace temperature is monitored ing them in holes drilled in the sample. For the temperature through a custom spark welded 0.125 mm Pt-Pt 13% Rh and the material evaluated, the results were consistent within bare wire thermocouple mounted in an extruded alumina+ twin the measurement uncertainty. bore tube and wrapped in a molybdenum radiation shield. Once the setpoint has stabilized, the thermal oscillations as observed from the furnace thermocouple are below 50 mK III. INSTRUMENTATION
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