Pd-C eutectic fixed point cells for a self-validating Type C thermocouple

O. Ongrai1-3, J. V. Pearce1, G. Machin1, S. J. Sweeney2

1

National Physical Laboratory, Hampton Road, Teddington, Middlesex, TW11 0LW, UK 2 Advanced Technology Institute, University of Surrey, UK 3 National Institute of Metrology (Thailand), Pathumtani, Thailand

The miniature Pd-C eutectic cell (1492 C) for thermocouple selfcalibration has been studied to transform the reliability of thermoelectric performance of the Type C thermocouple by facilitating in-situ calibration without need for removal sensor for recalibration.

Thermal environment effects

The emf at the melting plateau of the miniature Pd-C cell with varying furnace offset temperatures was studied to examine the influence of the ambient conditions.
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 The accuracy of high temperature measurement is significant in terms of: reducing product waste, minimizing energy consumption and promoting health and safety.  Thermocouples are the most widely used temperature sensor for high temperature measurement.  Type C (W5%Re/W26%Re) refractory thermocouples are almost universally used >1700 C.

Figure 2: The arrangement of the self-validating thermocouple. The thermocouple was fitted to the miniature Pd-C cell to make a self-validating device.

Thermocouple emf / V

1. Introduction

Integrated device

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1K

Furnace offset / oC

2. Metrology Challenge
 A new Type C thermocouple has a typical uncertainty of 1% of temperature (20 C at 2000 C) and this can rapidly and substantially increase with use.  Achievable accuracy is severely limited by homogeneity, drift, and hysteresis.  The removal of W/Re thermocouples after high temperature use is not possible due to embrittlement.  Thermocouples application is always different from the calibration situation. Hence, in-situ self-validation would significantly improve the use of type C thermocouples.

Measurement Furnace
Furnace supplier: Elite Thermal Systems Temperature range: 0-1800 C Work tube inner diameter: 12 mm
1340

Figure 6. The melting emf values as a function of the offset temperatures of the furnace. Error bars represent the type A uncertainty associated with each point (k = 1). The slope of the dashed line is 4.0 V/ C or 0.25 C / C. At zero offset, the emf is 26320 V 14 V.

5. Uncertainty
 In this case the thermoelectric inhomogeneity can be omitted from the uncertainty budget as the calibration is performed in-situ  This causes a very large decrease in the calibration uncertainty for the thermocouple
Uncertainty components Value Distribution
Repeatability emf / V Plateau determination / V Thermal environment / V Temperature of Pd-C / V Voltmeter calibration/ V Spurious emf / V Ice point uncertainty / V 2.3 1.0 4.0 5.8 0.5 0.5 0.1 Normal Rectangular Rectangular Normal Rectangular Rectangular Rectangular

1320

Temperature / C

1300

Standard uncertainty
2.3 0.6 2.4 5.8 0.3 0.3 0.1 7.0 14 0.9

1280

3. Measurement Set Up
Construction of a Pd-C miniature cell
 The crucible was constructed from pure graphite.  The pure Pd wire was repeatedly added and melted to fill the crucible (~ 4 g).  Dissolved graphite from the crucible formed a Pd-C eutectic.

1260 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35

Position / cm

Figure 3: Temperature profile (above) of a single zone vertical furnace (right) used to evaluate the quality of the device in a severe temperature gradient such as that in a typical industrial application. Here, uniformity over the central 50 mm is 4 C.

Combined uncertainty (k=1) / V

4. Results
Plateau behaviour
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Expanded uncertainty (k=2) / V Expanded uncertainty (k=2) / C

Table 1: Uncertainty budget of the miniature Pd-C fixed point cell using a Type C thermocouple.

Thermocouple emf /V

5K

6. Conclusions
 A miniature Pd-C eutectic fixed point cell was fabricated to evaluate the stability at ~1500 C of type C thermocouples by means of in-situ calibration.
Time / minutes

 The results show that the implementation of high temperature eutectic fixed points for self-validating W/Re thermocouples is possible.  This study shows that a step change improvement in high temperature thermometry is possible by mitigating the effects of sensor drift due to contamination and inhomogeneity.  Higher temperature eutectic fixed points and multiple fixed points in one crucible for thermocouple selfvalidation are both under development

Figure 1: (a) Cross-sectional drawing of the miniature graphite crucible. All dimensions are in mm. (b) The miniature graphite crucible in an upside-down orientation filled with small pieces of the palladium wire.

Figure 4: Repeated Pd-C melts and freezes of the miniature cell, measured with self-validating type C thermocouple.

Type C thermocouples
 Format: Mineral Insulated Metal Sheathed (MIMS)  Sheath: Molybdenum  Insulator material: Hafnia  Wire diameter 0.25 mm  Ungrounded measurement junction  Ice point reference

Repeatability
The emf of the point of inflection of the melting plateau, for a number of realisations of the Pd-C miniature cell.
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Thermocouple emf /V

References
avg.

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 Miniature metal-carbon eutectic fixed point cells for self-validating Type C thermocouples, Ongrai O, Pearce J V, Machin G and Sweeney S J, Measurement Science & Technology 22 (2011) 105103  Miniature Co-C fixed point cells for self-validating thermocouples, Ongrai O, Pearce J V, Machin G and Sweeney S J, Measurement Science & Technology 22 (2011) 015104  Self-validating thermocouples based on high temperature fixed points, Pearce J V, Ongrai O, Machin G and Sweeney S J, Metrologia 47 (2010) L1-L3
9786/0911 Queens Printer and Controller of HMSO, 2011.

0.2 K

No. of measurements

Figure 5: Repeatability of melting emf values of the miniature Pd-C fixed point cell. Error bars represent the type A uncertainty associated with each point (k = 1). The repeatability was 2.3 V or 0.15 C.

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