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4 - Ongrai

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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 self–calibration 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.
26355 26350

• 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 / μV

1. Introduction

Integrated device

26345 26340 26335 26330 26325 26320 26315 0 1 2 3 4 5 6 7 8

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 μV/ °C or 0.25 °C / °C. At zero offset, the emf is 26320 μV ± 14 μV.

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 / μV Plateau determination / μV Thermal environment / μV Temperature of Pd-C / μV Voltmeter calibration/ μV Spurious emf / μV Ice point uncertainty / μV 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

o

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) / μV

4. Results
Plateau behaviour
26450 26400 26350 26300 26250 26200 26150 0 10 20 30 40 50 60 70 80 90 100

Expanded uncertainty (k=2) / μV Expanded uncertainty (k=2) / °C

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

Thermocouple emf /μV

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.
26354 26352

Thermocouple emf /μV

References
avg.

26350 26348 26346 26344 26342 26340 26338 0 1 2 3 4 5

• 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 © Queen’s 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 μV or 0.15 °C.

www.npl.co.uk

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