In-situ Resistometry for Heat Treatment Monitoring and Control

Motivation

Superconducting wires containing a brittle A15 phase, for example Nb3Sn, must first be processed as a composite of more ductile components, the A15 phase being subsequently formed during heat treatment once the conductor had been deformed to its final dimensions. The heat treatment conditions and the detailed design of the wire cross-section strongly influence the resulting superconducting properties, but discovering the optimum wire design and heat treatment schedule for a given application is generally a matter of time-consuming and costly trial and error. The optimisation process also needs to be repeated when the requirements change - for example, a different operating temperature or a larger magnetic field - or to take account of processing restrictions (the maximum attainable heating rate, for example). Our work on interpreting resistance measurements, modelling reaction-diffusion and calculating resistances has the potential to significantly simplify the optimisation process.

Concept

The electrical resistivity of a composite material depends sensitively on the dimensions and distribution of each phase, and on the properties of each phase - their chemical compositions, crystal structures, defect populations and strain state. For a sample in which these properties are changing, for example a composite wire during heat treatment, this can provide useful information about the changes occurring inside the sample without disrupting processing. It is not possible to directly extract the structural changes of interest from the measured resistance, as this resistance depends on so many factors. However, careful modelling of the design of a composite wire and how that structure evolves during heat treatment can be used to calculate the resistance, and comparison of measurements with calculations (in the full knowledge of the heat treatment history) allows useful information to be extracted.

For bronze-route Nb3Sn conductors, modelling the evolution of the structure during heat-treatment requires a good understanding of the reaction-diffusion processes (informed by experimental measurements), as well as the thermomechanical behaviour of the composite. This modelling in itself allows for optimisation of wire designs and heat treatments without performing resistance measurements. Combining this with resistometry could provide a powerful technique for monitoring the formation of the superconducting phase non-invasively during reaction, for both research and production purposes. Additionally, a computer-controlled furnace system could be developed to adjust the heat treatment parameters directly on the basis of the measured resistivity, to optimise the properties of the wire for a given application. That is the ultimate goal of our research in this field.

In addition to the calculation and modelling requirements, we have needed to develop a procedure for the in-situ resistance measurements at high temperature. To ensure that we can measure small changes in the resistivity, we use a four-terminal alternating current (AC) technique, with a lock-in amplifier. Measurements are conducted in vacuum to eliminate oxidation effects and isolate the sample from external disturbances. The temperature is monitored using a type K thermocouple next to the sample, and both temperature and the potential difference across a measured length of the sample are continuously recorded with a computer. The temperature is controlled using a Eurotherm controller and a tube furnace. This can also be connected to the computer, allowing us to use this system not just for resistometric monitoring of reaction processes, but also for true computer-controlled reaction.

More details

Further details are available - please refer to the links below, and the list of publications at the bottom of the page.

Related materials

Related publications

Showing 8 publications related to in-situ resistometry in date order.
Links to online copies of these papers may require a journal subscription (personal or institutional).
2003
1 K. S. Tan, S. C. Hopkins, D. Astill, M. Majoros and B. A. Glowacki, In-situ resistance measurements of stabilised and unstabilised Nb-Sn-Cu-Ta multifilamentary conductors during reactive diffusion
Inst. Phys. Conf. Ser., No. 181 2306-2313 (2003) 

EUCAS '03: 6th European Conference on Applied Superconductivity, Sorrento, Italy, 14-18 September 2003

2 S. C. Hopkins, K. S. Tan and B. A. Glowacki, Modelling of resistivity changes in multifilamentary Cu-Ta-Nb-Sn conductors for monitoring the development of superconducting Nb3Sn layers during isothermal heat treatment
Inst. Phys. Conf. Ser., No. 181 2322-2329 (2003) 

EUCAS '03: 6th European Conference on Applied Superconductivity, Sorrento, Italy, 14-18 September 2003

2004
3 K S Tan, S C Hopkins, B A Glowacki, M Majoros and D Astill, In-situ resistance measurements of bronze process Nb-Sn-Cu-Ta multifilamentary composite conductors during reactive diffusion
Superconductor Science and Technology, 17 (4) 663 (April 2004) | DOI: 10.1088/0953-2048/17/4/017 
4 K. S. Tan, S. C. Hopkins and B. A. Glowacki, Influence of heating rates on in-situ resistance measurements of bronze process Nb-Sn-Cu-Ta multifilamentary conductor
Physica C, 415 (4) 179-188 (1 November 2004) | DOI: 10.1016/j.physc.2004.08.013 
5 B.A.Glowacki, S.C.Hopkins, K.S.Tan, H.Krauth, In-situ Resistometric Measurements of the Reactive Diffusion Formation Processes in Nb-based Conductors as a Technique for Jc Optimisation
Proc. Int. Workshop on Progress of Nb-Based Superconductors, eds. K. Inoue, T. Takeuchi and A. Kikuchi, NIMS, Tsukuba, Japan, 45-53 (2004) 

International Workshop on Progress of Nb-Based Superconductors, NIMS, Tsukuba, Japan, 2-4 February 2004

6 K.S.Tan, S.C.Hopkins, B.A.Glowacki, A.Kikuchi, T.Takeuchi and K.Inoue, In-situ resistance measurements of Nb-Al multifilamentary conductors by solid-state diffusion and RHQT processes
Proc. Int. Workshop on Progress of Nb-Based Superconductors, eds. K. Inoue, T. Takeuchi and A. Kikuchi, NIMS, Tsukuba, Japan, 162-170 (2004) 

International Workshop on Progress of Nb-Based Superconductors, NIMS, Tsukuba, Japan, 2-4 February 2004

2005
7 K. S. Tan, S. C. Hopkins, I. Pong, R. J. Stearn, B. A. Glowacki, A. Kikuchi, T. Takeuchi and K. Inoue, In-situ resistance measurements of RHQT processed Nb3Al Superconductors
IEEE Transactions on Applied Superconductivity, 15 (2) 3532-3535 (June 2005) | DOI: 10.1109/TASC.2005.849352 

Applied Superconductivity Conference '04, Jacksonville, Florida, USA, 2004

2006
8 K. S. Tan, I. Pong, S. C. Hopkins, B. A. Glowacki, A. Kikuchi, T. Takeuchi and K. Inoue, Monitoring of intermetallic phase formation in jelly-rolled Nb/Al multifilamentary conductors by in-situ resistometry
Intermetallics, 14 (4) 450-455 (April 2006) | DOI: 10.1016/j.intermet.2005.08.002