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Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz, Robert Lindner 6 November 2012

Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

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Page 1: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Self-Validating Thermocouples For in-situ calibration drift correction

Claire J Elliott, Jonathan V Pearce, Graham Machin

ESA-estec: Christian Schwarz, Robert Lindner

6 November 2012

Page 2: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

The UK’s national standards laboratory

Develop & disseminate UK’s measurement

standards, and ensure they are

internationally accepted

Founded in 1900

500+ specialists in Measurement Science

State-of-the-art laboratory facilities (>380!)

World leading National Measurement Institute

About NPL

1/17

Page 3: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Talk overview

Temperature measurement scale, and fixed-points

Limitations of thermocouples above 1100 °C

High-temperature fixed points

Concept of in-situ self-validation & implementation

Performance of self-validating thermocouples, up to 2300 ˚C

Overview

Further development & results

Industrial applications

Conclusions

2/17

Page 4: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Temperature measurement scale

Internationally agreed temperature

scale of 1990: “ITS-90”

Defined by a range of fixed-points

from…

The lowest vapour pressure point

of helium (-270.15 ˚C)

to…

The freezing point of copper

(1084.62 ˚C)

Further information: www.bipm.org/en/publications/its-90.html 3/17

Page 5: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Temperatures above 500 °C

There are only four temperature fixed points

defined by the ITS-90 above 500 ˚C:

• Freezing temp. Al 660.323 ˚C

• Freezing temp. Ag 961.78 ˚C

• Freezing temp. Au 1064.18 ˚C

• Freezing temp. Cu 1084.62 ˚C

Thermocouples provide the best uncertainties at

high temperatures (for contact thermometry)

How can we judge the performance of, and

calibrate contact sensors above 1100 ˚C ?

4/17

Page 6: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Limitations above 1100 °C

Lack of ITS-90 fixed points

W-Re thermocouples are commonly used

above 1500 ˚C

• Embrittlement

• Quickly exhibit thermoelectric drift –

typically 10 ˚C within 10 h of operation

• Recalibration often impossible

To address this issue, NPL are working in

cooperation with ESA-estec to develop an

innovative method of validating the

performance of high temperature

thermocouples in-situ

Further information: Brixy et al. High Temperatures – High Pressures 12, 625-631 (1994)

[After Brixy]

5/17

Page 7: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

High-temperature fixed points

Novel high-temperature fixed points (HTFPs)

Many eutectic metal-carbon alloys have been

shown to be suitably stable as HTFPs, for

example:

• MP Fe-C 1153 ˚C

• MP Co-C 1324 ˚C *

• MP Pd-C 1492 ˚C

• MP Rh-C 1657 ˚C

• MP Pt-C 1738 ˚C *

• MP Ru-C 1953 ˚C *

• MP Ir-C 2292 ˚C *

• MP Re-C 2474 ˚C

• …

MP determined by radiation

thermometry

Reproducibility of the melting

point is known to be better than

±0.05 ˚C (k = 2)

6/17

Page 8: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Calibrations above 1100 °C

Co-C (1324 °C) & Pd-C (1492 °C)

HTFP construction:

Extremely pure metals

Graphite crucible – easy to manufacture

Tall for good immersion

Furnace:

High temperature furnace

Inert atmosphere (argon)

Measurement:

High temperature thermocouples

Materials compatibility issues

7/17

Page 9: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

In-situ self-validation

Overcomes embrittlement

Is a technique to check the calibration of a

thermocouple in-situ

The design consists of two parts:

• Miniature HTFP (containing a eutectic

M-C ingot)

• High temperature thermocouple

(Type C, W5%Re-W26%Re)

By incorporating a miniature HTFP cell onto

the thermocouple tip, the thermovoltage can

be verified each time the thermal environment

passes the fixed point transition temperature

8/17

Page 10: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Implementation

Thermocouple construction crucial – we would like to thank Omega Engineering

for supplying thermocouples with a customised design

9/17

Position the HTFP onto the

thermocouple in-situ

Observe thermocouple output

through the transition temperature

Apply suitable correction algorithm

to the output reference function

Assured measurement

confidence and

extended useful life

Choose a HTFP – with a transition

temperature to match process The user is enabled to

perform a suitable

adjustment to the

reference function

(can be automated)

Page 11: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Prototype Test Arrangement

HTFP cell positioned on Type C thermocouple

Thermal cycling

• Ramp rate of 1 ˚C/min

• Held at maximum temperature for 1 hour

• Presence of cell does not impede sensor

function (under these conditions)

Melting temperature assigned by radiation

thermometry (ISO17025, traceable to ITS-90)

10/17

HTFP alloy Melting temperature,

°C

Uncertainty

(k = 2), °C

Co-C 1323.28 0.64

Pt-C 1737.52 0.94

Ru-C 1952.98 1.00

Ir-C 2289.70 1.56

Page 12: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

11/17

Performance

The performance of the four self-validating thermocouples:

Page 13: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

11/17

Performance

The performance of the four self-validating thermocouples:

At high temperatures, the thermocouple reading is clearly unreliable

Page 14: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

11/17

Performance

The performance of the four self-validating thermocouples:

At high temperatures, the thermocouple reading is clearly unreliable

Ru-C drift between 1st and 2nd melt is: 20.9 μV (~1.7 ˚C)

Page 15: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Overview

By correcting for every step in drift, the user gains confidence in the

temperature reading

• The thermocouple is kept within calibration: extending its useful life

• The uncertainty due to changing thermoelectric homogeneity is eliminated

Design and use can be tailored for specific requirements

Development areas:

• One ingot (fixed-point temperature) and therefore limited temperature

range of correction validity

• Short term exposure

• Ingot size

• Thermocouple and HTFP cell are separate items (at present)

12/17

Page 16: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

First multi-cell results

Multi-cells to allow dual validation; contains both Pt-C and Ru-C

Each ingot is clearly observed, therefore

Good thermal contact has been achieved 13/17

Page 17: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

14/17

Extended exposure

Extending the exposure to 10 h at high temperature:

Maximum temperature maintained for 10 hours

Thermovoltage drift over 5 h (at Ir-C) is 347 µV, equivalent to ~43 ˚C

Page 18: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Industrial applications

Benefits to industry are clear

• Improved temperature measurement and reliability

• Casting / Manufacturing – reduced costs and enhanced quality

Looking to develop into a commercial device

• User requirements

• Develop correction algorithm

Nuclear industry – self-validation with low neutron

capture cross-section materials e.g. Fe-C and Cu

(EMRP project “MetroFission”)

15/17

Page 19: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

Conclusions

The thermocouple and HTFP arrangement has been

shown to be suitable for self-validation

• Cell size provides suitable immersion

• The presence of the cell does not impede on

the function of the sensor, under these

conditions

Application of in-situ self-validation will achieve:

• Assured temperature measurement confidence

• Extended useful life of the sensor

Which opens up the possibility for:

• Improved temperature measurement /reliability

• Reduced costs and enhanced quality

16/17

Page 20: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

www.npl.co.uk/temperature-humidity

Email: [email protected]

Thank you…

…for your attention

Page 21: Self-Validating Thermocouples...Self-Validating Thermocouples For in-situ calibration drift correction Claire J Elliott, Jonathan V Pearce, Graham Machin ESA-estec: Christian Schwarz,

HTFP = 1323.28 ˚C ± 0.64 ˚C HTFP = 1737.52 ˚C ± 0.94 ˚C

HTFP = 1952.98 ˚C ± 1.00 ˚C HTFP = 2289.70 ˚C ± 1.56 ˚C