Induction
Heating and the Floating Zone Method
The need for ultra-high purity
materials has led to improvements in the zone processing method of accurately
controlling the level of impurities and alloying elements within an otherwise
pure material. By heating a very small region of the material to be refined to
its molten state and controlling the movement of this zone, impurities can be
extracted from the solid material and collected by the molten or liquid zone. As
the molten zone traverses the source material and re-solidifies, the solidified
material will have a lower impurity level (dependent on alloying element). This
process can be repeated multiple times resulting in ultra-high purity materials.
Alternatively, zone processing can be used to control the level and distribution
of alloying elements in a given material. The use of induction heating in
the zone processing method offers several advantages over other heating methods.
By controlling the electromagnetic field, stirring can be induced in the molten
zone resulting in higher process efficiency. Additionally, through coil design
the heated zone length can be controlled and tailored for optimum efficiency.
Coupling the induction power supply with a closed loop feedback circuit also
offers improved process control. Induction heating also enables the use of
controlled atmospheres, including vacuum, and non-contact heating or cold wall
chamber heating, which can further reduce the level of trace impurities.
Interest
in semi-conductor devices for operation at higher temperatures has stimulated
the production of high purity single crystals of silicon of known orientation.
Unfortunately, the high chemical reactivity of silicon and its high melting
point (1412°C) offer special problems with respect to zone processing. The most
practical solution to these problems has proven to be the floating zone
technique, and most of the very pure silicon produced today is processed in this
way. Since the floating zone method is capable of growing single crystals with a
given orientation, as well as zone refining and leveling, it is ideally suited
to the production of silicon crystals for semiconductor devices.
Much recent
work in the technology of silicon production has been directed toward the
development of single crystals of larger diameter. The fundamental principles of
the floating zone method, however, pose practical limitations to the diameter of
bar which can be successfully processed. These limitations indicate that the
maximum diameters processed depend significantly upon the ability of the
processing equipment to maintain a narrow liquid zone.
FIGURE 1 shows a
power supply used to successfully process bars of silicon up to 1-1/4 inches
(31.75 mm) in diameter.
This equipment consists of a Lepel 15 kW, 2.5 to 5
MHz, three-phase (T-15-3MC) induction heating generator, a remote tank assembly
with matching transformer, and a single-turn induction heating coil.
The generator
shown in FIGURE 1 operates at a frequency of 2.5 to 5 MHz using a single-turn
coil and the matching transformer. Saturable core reactors are located in the
input of the generator to minimize D.C. ripple and to provide smooth and
noise-free power control. In addition, ripple filter capacitors may be placed
between the R.F. filter capacitor and ground to further reduce D.C. ripple.
Continuous power control is achieved manually by operation of a powerstat placed
in the primary to control the saturable core reactors. Remote power control can
be accomplished through a 4 - 20 mA analog input signal or digital serial port
connection. The serial port connection also enables remote monitoring of
critical power supply parameters.
FIGURE 2 is a close-up of the remote tank assembly
with built in matching transformer. The transformer has a multiturn water-cooled
primary and a single-turn skirt secondary, also water-cooled and grounded. The
induction coils can be tailored for the specific application.
Using the
equipment shown in FIGURES 1 AND 2, a liquid zone can be moved along the silicon
bar to produce a uniform bar of high purity. FIGURE 3 shows the liquid zone in
the silicon bar during processing.
| In processing a raw silicon bar to
produce a single crystal of desired orientation, the bar can be preheated using
either a small molybdenum wire coil or carbon susceptor at one end to initiate
induction heating. The molybdenum wire or carbon susceptor, which heats readily
by induction and in turn heats the silicon, is placed in close proximity to the
silicon rod, making the silicon sufficiently conductive to thereafter be heated
directly by induction. The preheated silicon source rod and a monocrystal seed
are placed in proper position relative to the coil after preheating. After
heating one end of the polycrystalline bar to a high temperature, a molten zone
is produced at the polycrystal-seed interface. In operation, the silicon bar is
moved through the coil while rotating; the solidified material forming a smooth
straight monocrystal having an orientation identical to that of the original
seed. Upon reaching the top of the polycrystalline bar, the power is reduced to
solidify the molten zone.
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FIGURE 4 shows a schematic of a typical floating zone set-up. While the
processing details for zone refining and growing single crystals of silicon vary
from plant to plant, the equipment and procedure described here have proven
successful for processing silicon rods up to 1-1/4 inches (31.75 mm) in
diameter.