SAMPLE LAB REPORT

(your report should be double spaced for grading purposes)

Introduction

For cast ingots, the size and shape of grains at any location is dependent on the solidification
process. The progress of solidification from the mold wall to the center of an ingot may occur in
three stages. Each stage is marked by a zone having a distinct grain structure. The three zones are
the chill zone, the columnar zone, and the central zone. The grain morphology (size and shape)
and the extent of each zone depend on the temperature of the molten metal, and that of the mold,
relative to the liquidus temperature of the alloy.

(Specific Discussion of Theory with Relevant Equations)

The goal of this laboratory is to determine how the pouring temperature of an alloy can affect the
grain structure of the ingot. Specifically, an Al-2.5% Cu alloy was used and the grain structures
obtained by pouring the alloy at two different temperatures were examined.

Procedure

Materials and Equipment

75 grams AA 6063 + 1.875 grams 99.9% Cu Al-2.5% Cu alloy

Furnace
Etchant - 1.0 ml HF (48%), 1.5 ml HCL (conc.), 2.5 ml HNO3 (conc.), and 95.0 ml H2O
Kellers reagent 75 ml HCL (conc.), 25 ml HNO3 (conc.), 5 ml HF (48%), and 35 ml H2O
Neophot 21 Metallograph
Steel crucible

Two samples of Al-2.5% Cu alloy were made, put into the furnace at 850C, and melted. They
were kept there for 20 minutes in order to obtain a constant temperature throughout both samples.

After 20 minutes, sample A was taken out of the furnace and poured into a steel crucible which
was at room temperature. The other sample, Sample B, was allowed to solidify without being
poured. It was then put into a furnace at 690C and remelted. Sample B was also kept in the
furnace for approximately 20 minutes and then poured into a steel crucible. Each sample was
allowed to cool and solidify.

Each sample was cut down at its central axis, and then ground and polished according to standard
metallographic procedures. Each sample was then etched with the enchant solution, in order to
obtain its microstructure.

After examination with the Neophot 21 Metallograph the samples were etched again using the
Kellers reagent, so as to obtain the macrostructure for each.

Results

(Opening Statement: General trends found in the results)

After examining Sample B with a magnification of 25X, it was determined that it has an equiaxed
grain structure in its middle with a chill zone around its sides where the metal had been in contact
with the crucible wall. A few dendrites were observed at the very top of the sample oriented
towards the center of the sample. Photographs of the equiaxed structure in the middle of the
sample and of the chill zone at the base of the sample are given in Figure 1.

Figure 1: Microstructure of Sample B - Equiaxed Structure and Chill Zone at 25X

The microstructure of Sample A was also examined with a magnification of 25X. As

shown in Figure 2, it was observed that the sample poured at 850C also had a chill zone around
the edges of the sample. However, the microstructure in the middle consisted of columnar grains.
The long dendrites viewed were basically all oriented towards the middle of sample.

Figure 2: Microstructure of sample A - Chill Zone at 25X

It was observed that both samples were very porous. Each sample had relatively large
irregularly shaped pores throughout the observed section. An example of the pores can be seen in
both Figures 1 and 2.

Discussion

The purpose of this laboratory was to study the effect of the pouring temperature of the liquid on
the grain structure of the solid alloy. Sample B was poured at a temperature close to the freezing
temperature of the alloy. The pouring temperature of the sample was 690C while the freezing
temperature was approximately 660C. This is the primary reason why Sample B had an equiaxed
grain structure.

The same is true of Sample A. The columnar grain structure is a direct result of its pouring
temperature. The pouring temperature of sample A was 190C above the freezing point of the
alloy.

In Sample B, the equiaxed grain structure obtained was due to the pouring temperature. The
liquid alloy was allowed to stabilize at a temperature before being poured into the steel crucible.
The temperature of the liquid was approximately 30C above the freezing temperature. When the
liquid was poured into the crucible, which was at room temperature, the liquid alloy that touched
the side walls of the crucible solidified.

Solid nuclei formed heterogeneously on the walls of the crucible. As the nuclei began to grow in
preferred directions the protrusions intercepted each other. As each protrusion grew, they began to
run into each other and stop growing. The conglomeration of nuclei whose growth was stunted
was called the chill zone. This chill zone can be seen in Figure 1. However, some protrusions that
were oriented towards the center of the crucible were not intercepted by other protrusions and,
therefore, continued to grow. The equiaxed structure which formed in the middle of the sample
was due to protrusions of this type. These protrusions, which were developing into primary
dendrite arms, were, somehow during the pouring, broken off and swept into the middle of the
liquid alloy.

There are two possibilities as to how the protrusions were broken off. The first possibility is that
the turbulence in the liquid, as it was being poured, broke the protrusions off. The second
possibility is that as the mould walls increased in temperature the base of the protrusion was
remelted without melting the rest of the protrusion, in that manner, the solid nuclei was allowed
to mix with the rest of the liquid.

Since the pouring temperature of the liquid was so close to the freezing temperature, the solid
nuclei that were swept into the middle of the liquid did not melt. The temperature of the liquid
was not high enough to remelt the solid nuclei. Therefore, the solid nuclei provided heterogenous
nucleation sites for the rest of the liquid to nucleate on. These particles began to grow in every
direction through the development of protrusions. These protrusions could not develop into
dendrites because the material was solidifying from both the inside and the outside. The
protrusion could not grow for very long in a preferred direction before they ran into other
protrusions which stopped their growth.

Due to the larger volume of space in between particles, however, the equiaxed grains were
allowed to grow larger than the chilled zone grains. This difference in size can be seen in Figure
1.

The few columnar dendrite grains at the top of sample B were due to the fact that there were not
any particles near the top to stop the growth of the protrusions. Therefore, they developed into
dendrites. The protrusions which were swept into the center of the liquid may have sunk more to
the bottom of the crucible. In that case they would not have been near the top to prevent the
columnar growth.

Sample A developed in the same manner as Sample B as far as the chill zone was concerned.
However, when protrusions were broken off, whether from turbulence or melting, they were
remelted when they were swept into the liquid. For sample A, which had a temperature 190C
above the freezing temperature, as shown by the phase diagram, none of the protrusions could
remain solid. Due to the high pouring temperature of the liquid the protrusions were remelted.

Because of the high pouring temperature, Sample A developed columnar grains. The columnar
grains were due to dendrite formation in preferred directions. The dendrites formed because of
the stead removal of heat through the mould walls. Those protrusions which were oriented
towards the center of the sample grew in the direction opposite to the flow of heat. Since heat was
removed in every direction away from the mould walls, all of the dendrites formed in a direction
pointing towards the center of the sample.

Solid nuclei developed heterogeneously along the walls of the crucible forming a plane of solid.
As the temperature of the liquid began to cool and approach the freezing temperature given of the
phase diagram the plane of solid began to grow. As temperature gradients moved through the
liquid some parts of the solid plane were surrounded by a cooler liquid than others. This variation
in temperature allowed some of the solid in the solid plane to grow and form faster, thus
producing protrusions. These protrusions were allowed to grow as the liquid became cooler and
cooler.

The development of dendrites occurred when the protrusions became very long and began to
develop secondary arms. The formation of the dendrites was opposite to the direction of heat
flow. The heat flow outward in all directions around the crucible made the dendrites grow
towards the center of the crucible.

Columnar grains are made up of several dendrites. All of the dendrites must have the same
preferred orientation. This leads to the columnar grains being oriented similarly. Therefore, the
columnar grains should also be pointed in the direction opposite to heat flow, or rather, towards
the center of the crucible.

One final point about the structure of both ingots was the pores that developed when the liquid
solidified. The pores were mainly due to shrinkage. When the liquid solidified, it shrank. The
dendrites formed by protruding out into the liquid where they shrank leaving more space for the
liquid to occupy; however, there was less liquid because the dendrites were forming. The liquid
that remained was all that was left to fill in the spacing between the dendrite arms. This liquid
when it solidified also shrank leaving large holes in between the dendrites. The result was a large
number of pores throughout the structure of the ingot. An example of the pores can be seen in
Figures 1 & 2.

Conclusion

(Key Observations/Conclusions Relevant to the Goal)

In conclusion, it was determined that the pouring temperature for casting and for making
ingots controls the grain structure of the final solid.

References

Phase Transformations in Metals and Alloys, Porter and Easterling, Van Nostrand Reinhold,
Berkshire, England, 1981.

Effect of Pouring Temperature on Grain Structure, Materials Department, Mat. E. 3084, Lab
Report, 11/29/89