Investigation of fixed points in monotectic alloys

Darsh Kodwani
National Physical Laboratory, Hampton Road, Teddington, TW11 0LW, UK Email: darsh.kodwani.2011@live.rhul.ac.uk

Introduction
Temperature metrology relies heavily on the concept of fixed-points physical phenomena, mostly melting or freezing, that occur at welldefined and unique temperatures. Fixed points greatly aid standardisation of measurements and can be used as checks of calibration. NPL has previously looked at two aspects: 1.  Calibration checks of sensors by including a reference fixed point within the sensor itself. 2.  The possibility of fixed points using new alloys that provide more than one fixed point temperature within a single ingot of material. In this experiment a furnace heated and cooled the fixed-point / thermocouple assembly, and transitions (seen as plateaus in a temperature-time plot) identified. These results were analysed to see if the transitions are stable.

Zinc-Bismuth crucible 1
The powders of Zinc and Bismuth were mixed together in the quantities: Zinc mass = 1.47 g Bismuth mass = 9.24 g Once again the same problem of being able to sink in the metals to be able to fit everything is was present. After heating the powders from the first fill, the powders had not melted and the crucible was used as it was. The weight of the constituents in the crucible was 7 g.

Aluminium-Indium crucible 1
This crucible was filled using aluminium and indium in powdered form. The powders were mixed together in relative mass proportions that gave a 1:1 atomic ratio between aluminium and indium. The masss used were: Aluminium mass = 1.16 g Indium mass = 5.2 7g The crucible was then filled with as much powder as possible, since the powder will take up more volume than a liquid. The idea was that the powder would be heated above the melting point of both aluminium and indium and therefore one would expect that the powders would melt and sink to the bottom once liquefied. However, when the crucible was heated, the powders did not melt and sink to the bottom. The process of heating was attempted several times, but the result did not change. This might be because of the surface tension of the liquids, so that even once they had melted, the structure remained the same. A simple solution to this problem is to simply disturb the crucible once it was in the furnace (a lot easier said, than done when the furnace is at 700+C). As the metals did not mix with each other, multiple features in the melt and freeze curves were observed, corresponding to the individual metals (as supposed to the alloy).

Aluminium-Indium crucible 2
This graphite crucible was filled with solid chunks of indium and aluminium powder. This time the method to try and get all of the contents inside the crucible was different to the first one. The melting point of indium is only 156C, therefore this temperature could be reached by a powerful hot air gun and that is what was used. First chunks of indium were put in the crucible and melted using a hot air gun, and it is here that it became clear that the reason the powders were not sinking in the previous crucibles was indeed (as was suspected) the surface tension of the metals. It was observed that even after the temperature of the crucible and the metal had reached far above 156C, the chunks of indium remained in the same position. But a small disturbance to the crucible caused the indium chunks to liquefy and fall to the bottom!

Conclusion
The data obtained is promising, as it regularly gives indications of two fixed points (phase transitions) being present in a single crucible. The data obtained from the zinc-bismuth alloy, appears to be the more promising of the two alloys, whether this was due to poor execution in making the aluminium-indium alloy or the fact that the alloy itself does not work as expected, is up for debate. To conclude, more measurements over a longer period of time are needed to examine the stability of the alloys.

Phase diagrams
The phase diagrams here indicate monotectic alloys. With two invariant reactions in each diagram represented by horizontal lines (showing there is no change in temperature), both the alloys would be expected to show two phase transitions each.

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