PYL 701

Zone Refining Technique

[Entry No-2017PHZ8396]

SAHIN SORIFI
6/11/2017
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1. Introduction

Zone Refining is a method to purify materials by melting a Zone and causing

this liquid zone to travel slowly through a relatively long rod of the solid. Many
elements and thousands of Organic and Inorganic materials are purified by using
this technique. Most of the developments in Solid State electronics would have
stopped if the two elements Germanium and Silicon had not been produced in the
desired purity level. Many elements when brought to their highly purified form
exhibit some new properties, which opens up a
new area of research.

Zone Refining was discovered by Scientist William

G. Pfann.

2. Process of Zone Refining

This technique works on the principle that the

impurities have higher solubility in the molten metal Taken from: Zone refining by Shrey Singh

compared to that in the solid metal. This difference and Kartikay Agarwal

in the solubility of impurities makes it possible to

segregate the impurities in the metal to be refined.

For the process, a rod of impure metal is taken. This rod is placed in a tubular zone
refiner. Inside the refiner an inert gas environment is maintained. A circular mobile
heater is placed around the rod. This heater moves along the rod from one end to the
other. At a time, heater melts a particular zone or portion of the metal rod along with
its impurities. As the heater moves to the next zone of the rod the molten metal of
the previous zone gets solidified again. During solidification of the metal, impurities
of the zone move to heavily heated zone or the
zone that is in contact with the heater. In other
words, as the heater shifts from one zone of the
metal rod to another the impurities also shift to the
zone of the molten metal. By the time, heater
reaches to the other end of the impure metal rod,
the impurities get concentrated there. The end of
the metal rod with concentrated impurities is then Taken from:
removed and discarded. The same process is https://www.youtube.com/watch?v=ZAYA
e_Oimlo
repeated again and again till a highly purified metal
is obtained.
https://www.youtube.com/watch?v=ZAYA
e_Oimlo&t=13s
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3. Lever Rule

A tool which enables us to determine the relative amounts of two phases or

the weight percentages of two phases in a binary phase diagram.

The drawn figure is the

temperature vs composition
phase diagram. A tie line is
drawn from point O parallel to
X axis to determine the weight
percentage in solid and liquid
form for point O. The
following expressions
determine solid and liquid
weight percentages:

Weight percentage of solid phase = (W0-Wl)/(WS-Wl)

Weight percentage of liquid phase = (WS-W0)/(WS-Wl)

4. Explanation of Zone Refining using Phase Diagram

The Zone Refining process is

based on the fact that the solid to
crystallize first from the melt is
purer in A or the element to be
obtained than the liquid.

Here we apply the Lever Rule for

the basic understanding of
concept involved in Zone refining.

As shown in the diagram, it is an

enlarged view of binary phase diagram of two components, A and B. Let us consider
A to be the element to be obtained and B is the impurity. The liqudous and solidous
lines are marked and the uppermost region is liquid region, the middle one region is
the mixture of solid and liquid and the lowest region is purely solid.

Let us consider solidification of the material at initial composition Cs. Thus

solidification starts at temperature T1 and just below this temperature when it starts
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to solidify, a small quantity of solid of composition Cs’, purer than Cs in A separates

from the liquid. (Application of Lever Rule)

Now, the leftover solid is again remelted. We see that solidification gets started at
higher temperature T2 (>T1). Again, the obtained solid after this process is smaller in
quantity but purer in A than previous concentration. By repeating this sequence the
optimum number of times, we obtain very pure A, even though the quantity of A is
very less as compared to the initial concentration of the material. In Zone Refining
this principle of phase separation is used.

5. Ordinary Freezing and Zone Melting

Fig. taken from Zone

Refining by William G.
Pfann.

Both the processes change the distribution of solute in a solvent. In reality one-pass
zone melting is actually less effective as a refining method than normal freezing. It is
illustrated in the figure below.

Impurity distribution produced by normal

freezing and that produced by one-pass
melting are different. The curves are shown for
sample charges of the same initial
concentration of solute (C0) and the same
distribution coefficient (0.5). The amount of
solute, or impurity, in the newly formed solid
rises much more steeply in zone melting than Fig. taken from Zone Refining by William G.
in normal freezing. The virtue of zone melting Pfann.

emerges, however, when a molten zone is passed through an ingot many times.
Moreover, the flat region between a and b in the zone melting curve can be exploited
to produce an ingot whose content of a desired impurity is extremely uniform. This
process is termed Zone levelling.

6. New Zone Refining Techniques for Chemical Compounds

New and advanced tools are being utilized to make the organic and inorganic
compounds zone refined. Recently a new technology using heating process has been
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developed which uses regular convection in the liquid and a mild rotation of a
charged tube which is kept horizontally in order to attain zones which are small in
size, in tubes of moderate diameter. A cooling technique has also been developed
where the liquid coolant is directly connected with the charged tube to get short
interzone spacing and a flattened interface of liquid-solid. These two techniques are
efficient for both semiconductors and metals. Other applications such as single
crystal growing, natural freezing and zone leveling can also be performed using
these techniques.

7. Discussion

In this article a brief idea of the process of Zone refining has been given. The
Zone Refining process has been described using the concept of Phase Diagram. Later
on a contrast between ordinary freezing and zone melting was highlighted and lastly
a new zone refining technique has been briefly discussed.

References

1. G.Pfann,William. Zone refining. Scientific American. Vol.217,No-6(December

1967),pp. 62-75.
2. G.Pfann,William; Miller,C.E; Hunt,J.D. New Zone Refining Techniques for
Chemical Compounds. Review of Scientific Instruments,37,649( 1966 ).
3. Singh,Shrey;Agarwal,Kartikay. Zone Refining.10D110010,UG sophomore
year, Dept. of ME & MS.
4. https://www.youtube.com/watch?v=ZAYAe_Oimlo
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