Analyzing Sintering Properties of

Alumina Powder for Industrial

Applications

Peter Mueller

Lab Group WA2

February 4, 2015

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Abstract
This experiment was performed to determine the sintering properties of an
alumina powder, including green density, fired density, porosity, and linear
shrinkage, and to use these properties to recommend a design and procedure for
creating a beam out of alumina. 0.55 g samples of the alumina powder were
measured, pressed into cylindrical pellets by a 2000 lb load, and fired for various
durations at 1400C, with the physical dimensions of the samples measured during
every step. It was found that the procedure used gave a green density of 2.25
0.05 g/cm3, and that fired density and linear shrinkage varied with firing time. It
was determined that sintering for 0.3 hours gave the best combination of high
density and limiting of grain growth. At this sintering time, the fired density was
extrapolated to be ~3.63 0.09 g/cm3, porosity was found to be 9.25%, and linear
shrinkage was found to be 15.3%. These results were found to be extremely
reproducible, with green densities only varying by 2% and fired densities varying by
3 to 4%, depending on the firing time. These sintering properties were investigated
to assist in designing a process for creating a cantilever beam. The dimensions of
the beam are to be 0.4 x 0.4 cm in cross-section and 5.5 cm long and the beam
must be able to support a 50 g load at 5 cm with no more than 4 m of deflection.
Based on the linear shrinkage values determined, a process for creating this beam
was designed, with a die pressing down perpendicular to the long axis and mold
interior dimensions of 0.48 cm x 0.48 cm x 6.6 cm. The next step for the company
is to test this configuration for green and fired density consistency as well as
accurate linear dimensions.

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Table of Contents

Introduction
Experimental Procedure

Results and Analysis

Design

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Recommendations

11

Appendix A

12

Appendix B

12

Introduction
Sintering of ceramic powders is an important method of producing solid
ceramic structures, such as disk brakes or knife blades, in science and industry
(Francis 2). Sintering is the process of forming a solid mass of material by
compacting a powder and heating it to a temperature below the melting point of the
material. The main motivations for using sintering instead of other processes is that
it requires lower temperatures than melting, allows for better grain size control than
melting, and can more easily be made into specific shapes than some other
methods (Sintering). These properties make sintering a logical processing method
for manufacturing small, precise parts. This experiment was conducted to gain a
better understanding of a specific sintering process for the production of a small
cantilever beam.
To understand the utility of sintering, it is necessary to understand the
process by which it occurs. The first step of sintering is the creation of a suitable
powder. Control of granule size in a powder is extremely important, as extremely
fine powders (e.g. silt or powdered sugar) do not flow well, while very coarse
powders (e.g. gravel) leave large voids in their macrostructures. The maximum
theoretical density of a randomly arranged grouping of spherical particles is roughly
64%, but this can be improved greatly by creating powders with multiple different
particle sizes (Scott). This allows the small particle size which fills voids tightly
while also giving the good flow characteristics of large granules. Typically, a binder
is used in sintering powders to give even the powder even more tunability. Binders
are used to clump together a collection of extremely small particles into larger
granules. In a sintering powder, this allows for all of the ceramic particles to be
uniformly small but bound together into larger, more flowable powders for use in
molds. Under compression, these granules are broken up and the binder is burned
away during firing, leaving behind a uniform and dense ceramic solid.
The next step is pouring the powder into the die and compressing it. If the
die is complex, extra care must be taken to ensure even distribution of the powder
in a die. Compaction of a powder in a die occurs in three steps (Francis 2). The first
step is the granules rearranging themselves to reach a more favorable
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conformation. This step is hindered by the friction of the walls of the die and by the
friction between granules. The second and most important step is the deformation
of the granules. The binder is chosen to be mechanically weaker than the base
material being compressed, which means that under compression, the binder will
yield first. This allows the powder to initially flow like a larger grained powder, but
then allows it to be compacted into spaces on the order of the smallest particle.
The final step of compression is the actual ceramic particles being deformed

(a)

(b)

(c)

elastically and plastically. This step should be dealt with with care, as leaving too
much elastic strain in the matrix while compressed can cause the green sample to
expand greatly or even crack when released from stress. These cracks are
significant because they could cause the green samples to break apart before being
able to be fired. Additionally, some of the cracks could remain on the inside of the
sample through the firing process, providing locations for crack formation and
growth in the fired ceramic, which would significantly weaken the final product.
Figure 1 shows the microstructural characteristics of the three stages of powder
compression.

Figure 1. Micrograph of alumina powder undergoing compression. (a) loose state,

(b) initial alignment stage, (c) plastically deforming final stage (Compaction)
After compression into a green solid, the ceramic is ready to be sintered, or
fired. The purpose of firing the solid is to raise the material to a temperature
where it does not liquefy, but the thermal energy is high enough for significant
diffusion to occur, allowing the particles to rearrange themselves into a more
thermodynamically stable conformation, which almost always has a higher density
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than the green density. Initially, as the temperature rises, the binder burns off, as it
is typically made of a polymeric material (Gupta). This is important, as it leaves a
pure ceramic and allows for the ceramic to achieve higher densities. As the
temperature approaches and reaches the sintering temperature, typically around
2/3 the melting temperature of the ceramic, the thermal energy reaches the level
needed to create large numbers of vacancies and to initiate certain atomic or
particle rearrangements. The driving force behind the sintering process is
thermodynamics. All boundaries between two different materials have a surface
energy and thermodynamics seeks to minimize this free energy in the system. In
the case of sintering, a ceramic-air boundary typically has a higher surface energy
than a grain-grain boundary, which causes thermodynamics to push towards the
elimination of ceramic-air boundaries. Additionally, due to the geometry of a
powder compact, compaction typically causes more ceramic-air boundary to be
removed than grain boundary to be created, which leaves less total surface areas.
These processes tend to push air and void space out of the material, as voids
contribute only surface area to the compact and are thus thermodynamically
unfavorable. This elimination of void space is known as densification, as it leads
to the ceramic taking up more of the volume of the solid and causes the density of
the solid to rise. Densification is desired because voids add nothing to the
mechanical strength of the material; denser materials typically exhibit the same
level of strength in a smaller volume. This gives a stronger overall material,
allowing either for a smaller design or greater strength for a specific part. The
microstructural changes associated with sintering at four different time lengths are
shown in Figure 2.

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Figure 2. Microstructure of a ceramic sample during sintering. (a) powder compact,

(b) initial sintering, (c) intermediate stage showing significant diffusion, (d) final
stage showing void reduction (Francis 2)
The competing process to densification is known as coarsening. Coarsening
is another thermodynamically favorable process in which material from one or more
grains jump across grain boundaries to add to larger, growing grains. This is an
energetically favorable process because the surface area to volume ratio for shapes
goes down as the shape gets bigger and surface area is typically an energetically
negative phenomenon. This increase in grain size typically has a negative effect on
the final properties of the material, as grain boundaries act as barriers for
dislocation motion, strengthening materials. Thus, a balance between time and
temperature should be chosen to maximize densification while limiting grain
growth. One way to do this is to not sinter a sample any longer than it needs to
reach the desired density, as once the density goal is reached, any extra time will
only worsen mechanical properties.

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After sintering, the sample is allowed to cool down to a safe temperature,

during which time shrinkage typically occurs. Any material undergoing an increase
in density while keeping the same mass must necessarily decrease in volume. This
decrease in volume can be represented by three linear shrinkage values, one for
each dimension. Linear shrinkage is calculated as L/L0, where L is the change in
length of the dimension and L0 is the original length of that dimension. If the green
solid is created without large density gradients, the linear shrinkage should be
largely isotropic. Knowing the shrinkage allows for the dimensions of a die to be
increased so as to leave a correctly-sized part after shrinkage. The equation used
for this is,
Required Dimension =

Desired Dimension /(1

L
).
L0

(1)

As noted previously, the strength of a sintered ceramic will vary with its fired
density. To design a ceramic part using sintering, this relationship must be known.
One equation found to model this relationship for sintered alumina is given by
E = 410e-3.96P,

(2)

where E = elastic modulus of the alumina and P = volume fraction of pore (Francis
1). The volume fraction of pores can be determined by comparing the fired density
to the maximum theoretical density of the alumina, where

fired

.
P = (1-
theoretical

(3)

Using these relationships, the elastic modulus of a fired alumina sample can be
accurately predicted, allowing for an adequate firing time to be determined to
create a part to meet specifications.

Experimental Procedure
A Ceralox alumina powder was used in a sintering process to create solid
alumina pellets (Francis 1). Initially, the pressing die was cleaned with lab wipes
and WD-40 to remove any impurities or residual alumina powder that could affect
the final mass or cause damage to the die. The desired amount of alumina powder,
0.55 g, was measured out on a Mettler MS303s scale with a precision of 0.001 g,
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with a piece of paper used to transport the powder (MS). The 0.55 g value was
determined by multiplying the volume of the 1.27 cm diameter (diameter of the
die), 2 mm thick pellet by the maximum density (4 g/cm 3) and the maximum
theoretical packing density of 55%. The die was then put together, with the bottom
plug being inserted with the flush side up, to form the pellet cavity. Another sheet
of paper was curled into a funnel to direct the powder directly into the die with
minimal spillage and a cotton swab was then used to brush any residual dust off of
the inner die walls. The top of the die was put in and the die was placed into a
hydraulic press for compaction. The die was compressed at 2000 lbs. for 30
seconds, followed by a 20 second gradual release of the pressure. The pellet was
removed from the die, weighed as before, and the diameter and thickness were
measured using a General model 147 hand calipers with a resolution of 0.01 mm
(147). The pellets were then fired with the temperature first rising at 5C/min to
500C, then at 10C/min to 1400C, the final sintering temperature. Four pellets
each were held at this temperature for 0 (immediately cooled), 0.1, 0.6, and 1.2
hours, respectively, before being cooled to under 100C over a period of 3-5 hours.
Finally, the sintered pellets were again weighed and their diameter and thickness
measured. Additionally, there was a sample of double mass, 1.1 g, produced using
the exact same procedure and sintered for 1.2 hours.
General lab safety procedures were followed in the lab; specifically, safety
glasses were worn at all times to prevent eye injuries, and care was taken to avoid
unnecessary inhalation of alumina powder fumes, which could potentially cause
minor respiratory irritation.

Results and Analysis

An important topic of analysis for any production process is the
reproducibility of the results. In this process, the imprecise nature of doing the
measuring and die-filling by hand means that this is the step of the process most
likely to suffer from reproducibility problems. To examine the consistency of the
green pellet production process, the mass, thickness, diameter, and from these the
green density, were measured or calculated. The student t-distribution multiplier of
2.131, corresponding to the 16 pellets measured was used to generate 95%
confidence intervals for each characteristic, and the results are given in Table 1.
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Table 1. Green pellet 95% confidence intervals for mass, thickness, diameter, and
calculated density
Characteristi

Lower Bound

Mean

Upper Bound

c
Green Mass

0.501

0.528

0.555

(g)
Thickness

1.75

1.83

1.91

(mm)
Diameter

12.69

12.76

12.83

2.20

2.25

2.30

(mm)
Density
(g/cm3)
(calculated)

These calculations show that the density of the green pellet will be accurate to
within 0.05 g/cm3, or roughly 2%, of the mean 95% of the time, which is an
excellent result given the handmade quality of the process. Additionally, the
individual measurements showed that for the 16 samples produced, the average
deviation from the mean was less than 1%, showing a similarly tight distribution of
results. It was determined that random error dominates in this experiment, as the
random error dwarfed systematic error, even with 16 samples being tested. The
sources of systematic error were the starting mass of the powder, the green mass,
and the pellet thickness. Both of the mass measurements were accurate to within
0.001 g and the hand calipers used to measure the thickness of the pellet was
accurate to within 0.01 mm. To reduce the error on the thickness measurements,
the thickness of each pellet was measured 3 times and averaged to determine a
final value. As noted, the combined error from these three systematic error sources
was vastly lower than the random error present in the experiment. The parameter
most responsible for the variations in measurement was the thickness of the pellet,
which was dependent on the overall mass placed in the die. This makes sense as
the diameter of the die is fixed, causing any variations in total volume to be
accounted for in the thickness of the pellet. There was no discernable correlation
between starting mass and pellet thickness for the 0.55 g samples, likely due to the
extremely small differences in starting mass. Overall, this is an issue for sizing the
individual sample, but had no noticeable effect on density. This can most clearly be
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seen on the double weight sample, which was produced following the exact same
specifications except double the mass of powder. The pellet of this sample had
roughly double the thickness and double the mass of the normal pellets but had the
same density, being less than 1% less dense than the mean. This result is actually
closer to the mean than many of the normal pellets, showing that the overall mass
or thickness of the sample has little effect on the density after compaction. It was
expected that the double mass sample would have a density equal to or slightly less
than the other samples, as the H/D ratio increases, decreasing the effective load on
the die as frictional losses increase. In this case, the H/D ratio was still relatively
low, so the lack of a difference in density is not surprising.
In general, green densities for ceramics are typically in the range of 55% to
65% of theoretical density (Schoenberg, Sun). Specifically for technical alumina,
the maximum green density falls in the 55% of theoretical density range, and at the
pressure used in this experiment (roughly 70 MPa), it is closer to 53% of theoretical
(Francis). In this experiment, the average green density was found to be 2.25
g/cm3, which is 56.25% of the 4 g/cm 3 density of alumina (Bodiov). Thus, the
procedure used in this experiment produces a green compact with a density on the
low side of the average ceramic range, but on the high side of the range for alumina
powders. The manufacturer of the alumina powder used also gives typical green
densities, which fall in the range of 2.05-2.24 g/cm 3, lower than the experimental
result. This is an especially good result considering that the compressive force used
was not particularly high on an industrial scale and that alumina is an extremely
hard 9 on the Mohs hardness scale (Aluminium). In general, increasing the pressing
force on the powder would likely increase the green density, but this method suffers
from diminishing returns and the green density is already within an acceptable
range. Thus, the current pressing method does not need to be changed to achieve
acceptable results.
After firing, the samples were again weighed and measured to determine the
fired density, mass loss, and linear shrinkage from the firing process. The fired
density and 95% confidence interval was determined at each sintering time and is
given in table 2.
Table 2. Density of sintered alumina powder samples for different sintering times
(g/cm3)
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Firing time (hours)

0
0.1
0.6
1.2

Lower bound
3.24
3.43
3.64
3.55

Mean
3.30
3.55
3.67
3.70

Upper bound
3.36
3.67
3.71
3.84

Additionally, Figure 3 shows density plotted against firing time to show the
diminishing returns of density as firing time increases. It is clear that the density of
the finished ceramic rises as the sintering time goes up, but this process slows
considerably past roughly 0.3 hours.

Fired Density vs. Sintering Time

3.8
3.7
3.6
3.5
3.4

Fired Density (g/cm3)

3.3
3.2
3.1
-0.2

0.2

0.4

0.6

0.8

1.2

Firing time (hours)

Figure 3. Fired density vs sintering time. Four samples were created and sintered at
each sintering time
The mass lost by the pellets during the sintering process was 0.015 0.001
grams, which is 2.84% of the original average pellet mass of 0.528 g. The
thermogravimetric analysis of the powder given in the design memo showed a mass
loss of ~ 3%, which matches quite closely the mass loss as a percentage of the
original pellet mass (Francis 1). Thus it is likely that almost all of the mass loss is
attributable to the burning off of the binder, which is well understood and not a
problem for fabrication.
The after-firing measurement of the samples yielded interesting insights into
the properties of die molding. A notable feature of this data is the much larger error
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range for the thickness measurement than the diameter measurement, as can be
seen in Table 3. This is a result of the diameter of the mold being fixed, while the
thickness was a function of the volume of powder put into the mold. Any difference
in initial powder volume was taken up as a thickness difference, leading to
significant error range, while the diameter was essentially unchanging, leading to
almost no error at all.
These diameter and thickness measurements taken in the lab allowed for the
linear shrinkage to be determined. The values found are given in percentages in
Table 3.

As would be expected, the shrinkage was greater for longer sintering

times, as these longer times led to a larger overall shrinkage and a higher density.
An interesting note is how similar the thickness and diameter shrinkages are,
generally within 1% of each other, indicating that the material is essentially
isotropic. Knowledge of the shrinkage rates is key to designing a die for production
of a sintered ceramic part, as failing to account for shrinkage will lead to an
undersized part and incur significant retooling costs. It should be noted that the
shrinkage values are very variable and this must be taken into account when
designing a die to produce a specific part using these methods.
Table 3. Linear shrinkage of sintered alumina powder samples for different sintering
times
Diameter shrinkage (%)
Lower
Mea
Upper

Thickness shrinkage (%)

Lower
Mean
Upper

(hours)
0

bound
11.75

n
12.3

bound
13.03

bound
10.76

13.3

bound
15.96

0.1

13.90

9
14.4

15.06

12.74

6
15.6

18.51

0.6

15.47

8
16.0

16.71

10.99

2
15.4

19.87

1.2

16.14

9
16.4

16.73

14.16

3
15.7

17.38

Firing time

After firing at 1400C for 0.1 hours, the double mass pellet was found to have
a fired density of 3.68 g/cm3 and diameter and thickness shrinkages of 16.5% and
17.3%, respectively. The fired density much higher than the 0.1-hour average of
3.55 0.12 g/cm3, possibly due to the larger mass pushing down during sintering.
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The diameter and thickness shrinkages were also larger than the averages for 0.1
hours, indicating that the double mass pellet underwent significantly more
densification than the other pellets. This discovery could potentially be useful in the
design of the cantilever beam in that the beam creation setup could be designed to
be more like the double mass pellet than the other pellets. Specifically, the
sintering could take place with the beam oriented with the long side vertical, to
allow gravity to cause more compaction, which seems like the most likely
explanation for the greater density.
An SEM was used to image the surface of the sintered pellets to determine
surface properties, which are given in Table 4. To analyze the images, a small grid
was drawn on the surface on the same scale as the scale given in the image, and
the average value of each characteristic found was determined. The properties
found were average grain size, average pore size, and average pore content.
Table 4. Surface characteristics determined from analysis of SEM images
Firing time
(h)
0
0.1
0.6
1.2

Average Grain Size

Average Pore Size

Average Pore Content

(m)
0.25
0.32
0.53
0.81

(m)
0.51
0.44
0.29
0.12

(%)
72
61
33
4

Figure 4. SEM image of unsintered alumina sample, showing

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grid drawn on image to analyze surface properties

Figure 4 shows an example of the SEM images, with the grid drawn on to allow for
areal analysis. The average grain size was determined by estimating the size of as
many grains as could be clearly identified and averaging them. Average pore size
was done in the same manner, with pores generally being defined as the areas
between grains. Pore content was found by estimating the percentage of the top
plane made up of grains and subtracting from 100. All of these values were very
rough estimates, as the planes of the image are hard to discern and the grains are
irregular in size and shape.

Design
The memo for this experiment calls for the design of a beam to support a
cantilevered load without excessive elastic deformation. The required dimensions
for the beam are 0.4 cm x 0.4 cm x 5.5 cm and the beam must be able to support a
load of 50 g at 5 cm with no more than 4 m of vertical deflection (Francis 1). As
given in the design memo, the equation for deflection in a beam is

P L3
c=
3 E Iz

(2)

where c is the vertical deflection, P is the load, L is the distance from the support to
where the load is applied, E is the elastic modulus of the beam, and Iz is the polar
moment of inertia of the beam. Solving this equation for E given c = 4 x 10-6 m, P
= 0.4905 N, L = 0.05 m, and Iz = width*thickness3/12 =

2.133 x 10-11 m4,

gives a minimum E of 239.5 GPa. To effectively use this value in an engineering

application, the elastic modulus of a porous, sintered alumina sample must be
known. An equation for determining the elastic modulus of a porous alumina
ceramic is given,

E=410 e3.96 P

(3)

where E is the elastic modulus in GPa and P is the volume fraction of pores in the
sintered ceramic (Spriggs). Solving this equation for P using E = 239.5 GPa gives
the maximum volume fraction of pores to be 0.1358. This means that the sintered
alumina ceramic could be as much as 13.58% porous and still support the required
load without exceeding the maximum deflection. A sample of the fired alumina
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would have to be 86.42% alumina and thus have a density of 0.8642*4 g/cm 3 =
3.46 g/cm3 to meet the requirements of this cantilevered beam.
Figure 1, showing the relationship between sintering time and density of
samples, was used to determine an optimal sintering time for the cantilever beam.
As all of the samples sintered for 0.1 hours had a density comfortably above 3.46
g/cm3, a 0.1 hour firing time would be adequate to meet requirements. A longer
time makes more sense, though, as the modulus of the ceramic increases notably
beyond 0.1 hours. The curve begins to flatten out as time increases and shows less
than a 2% increase in density after roughly 0.3 hours sintering time. Thus, going
past 0.3 hours in an industrial setting would simply be wasting time and money.
Additionally, given that the heat up and cool down cycles take roughly 7 hours,
adding another 12 minutes to the process is a minor increase in processing time.
Given the 20% increase in elastic modulus and thus safety factor this increase
would bring for a 3% increase in manufacturing time, a sintering time of at least 0.3
hours is the best choice. It should be noted that 0.3 hours was not a tested
sintering time, so it is possible that sintering for 0.3 hours would not yield the
expected results. Thus, to confidently proceed with a 0.3 hour sintering time, it
would be wise to test this sintering time in a lab.
Designing a die to use in the pressing of the alumina powder for this
application requires another choice to be made. One option is a die 0.4 cm x 0.4 cm
x 5.5 cm with the pressing direction being parallel to the 5.5 cm axis. The other is a
die 0.4 cm x 0.4 cm x 5.5 cm with the pressing direction perpendicular to the 5.5
cm axis. The first option has the advantage of being simpler, requiring a smaller
press head and less consideration of evenly distributing the load, but would have a
much higher H/D ratio, likely leading to lower green and fired densities. A higher
H/D ratio leads to lower green density because a greater die height contributes
more wall friction, which opposes the compressive force, reducing the effective
compressive force. The second option would have a much lower H/D ratio and
would likely lead to higher green and fired densities, but would be more complicated
to create and use, as filling, pressing head size, and even load distribution would all
be potential issues. Despite these potential problems, the recommended die shape
is the second option, with the pressing direction perpendicular to the 5.5 cm axis.
This is because all of the experimental data from this exercise was gathered using a
die with a similarly low H/D ratio. Switching to a die with a value H/D > 10 would
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really require a new experiment to be conducted to confirm that adequate fired

densities could be achieved and would invalidate most of the work done up to this
point. Using the die with the pressing direction perpendicular to the 5.5 cm axis
gives an extremely high likelihood of being able to produce solid alumina with the
required density and thus strength for this application.
The final consideration for designing this beam is to take into account the
shrinkage of the beam during firing. Using 0.3 hours as the sintering time and
extrapolating the linear shrinkage values found experimentally, it seems reasonable
to use 15% shrinkage in all directions. The desired final dimensions must be
modified to take these shrinkages into account, giving,

Mold Dimension=

Design Dimension
1Shrinkage

(4)

It is considerably easier to machine off a small amount of material than add

material to a sintered ceramic, so it was decided to round up on mold dimensions.
Using Equation 4 and the shrinkages determined for a 0.3 hour sintering time, it is
found that the mold dimension should be roughly 1.2 times the design dimension
for each measurement. Multiplying the design dimensions of 0.4 cm x 0.4 cm x 5.5
cm by a factor of 1.2 gives final mold interior dimensions of 0.48 cm x 0.48 cm x 6.6
cm. The die, pressing down perpendicular to the 6.6 cm axis should have
dimensions of roughly 0.47 cm x 6.59 cm, to allow the die to move through the
mold without binding.
To replicate the conditions used during this experiment, a sintering time of
0.3 hours and a sintering temperature of 1400C should be used, as noted in the
experimental procedure. Given the mold dimensions and a desired green density of
2.25 g/cm3 to replicate this experiment, each mold should be filled with 3.42 g of
alumina powder. Also given the die dimensions and the 70 MPa desired stress
applied to the powder, again to replicate this experiment, the load that should be
applied to the die is 22,176 N or 4,985 pounds of force. Using these specifications
and the process outlined in the experimental procedure should produce materially
consistent samples that meet the design needs of the Alumina Corporation of
Minnesota.

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Recommendations
One issue that was noted during the execution of this experiment was that
simply using paper to load the powder into the die is not a very precise and clean
method. This leads to materials waste, inaccurate measurements, and most
importantly, die wear as spilled powder causes abrasion of the die. It would make
sense to create or purchase a funnel-type tool to direct the powder directly to the
bottom of the die without spilling or coating the inside walls of the die. To best
replicate the successful results of this experiment, it is recommended to use a die
with the pressing direction perpendicular to the long axis of the beam, as this
reduces the H/D ratio and helps with packing. As the current procedure gives a
green density of 2.25 g/cm3, at or above the typical range for alumina powders, the
current procedure or one similar to it should be used in the creation of the beam.
As was noted in the design, the most logical sintering time to use would be 0.3
hours at the sintering temperature, as this time reduces the risk of grain growth and
coarsening while giving most of the possible density increase. This sintering time
should first be tested in a lab to verify that it yields the expected results before
moving to production. Only one sintering temperature was tested, 1400C, and it
gave a resulting solid with more than adequate properties; as such, this
temperature can be left unchanged. This process gives a final solid with a density
of roughly 3.63 g/cm3 or 90.75% of the theoretical value for Al 2O3 and an elastic
modulus of 284.3 GPa, which is well over the required elastic modulus of 239.5 GPa
required to build the beam. Finally, it must be noted that the beam will shrink upon
sintering as the material densifies. This requires the die for the beam to be built
larger than the final beam to allow for this shrinkage. The dimension increase factor
was determined to be 1.2, giving die dimensions of 0.48 cm x 0.48 cm x 6.6 cm. If
the user wants to truly eliminate the chance of a beam being undersized, a
dimension increase factor of 1.2 or even higher could be used. The data collected
in this experiment shows that this process produces a material that meets the
product specifications and is consistent enough to justify moving forward. The next
step should be to create a die and mold in the specified size and test the same
parameters (green density, fired density) to prove consistency and create
specifications for scale-up to an industrial-scale process.

Mueller 18

Works Cited
Bodiov, Katarina; Pach, Ladislav; Kovr, Vladimir; eransky, Alojz. (2006),
Alumina Ceramics Prepared by Pressure Filtration of Alumina Powder
Dispersed in Boehmite Sol. Czech Silicate Society, http://www.ceramicssilikaty.cz/2006/pdf/2006_04_239.pdf
Compaction of Ceramic Powders. (2015), Wikipedia.org. Wikimedia Foundation.
http://en.wikipedia.org/wiki/Compaction_of_ceramic_powders
Francis, Lorraine. (2015) Sintering Lab Handout, Department of Materials Science
and Engineering, University of Minnesota-Twin Cities
Francis, Lorraine. (2015) Chapter 5, Powder Processes, Unnamed Materials
Processing Textbook
Gupta, Surojit; Green, David; Messing, Gary. (2010), Thermomechanical Behavior of
Ceramic Green Bodies During Presintering. Journal of the American Ceramic
Society, 93: 2611-2616. Doi: 10.1111/j.1551-2916.2010.03780.x
Schoenberg, S. E., Green, D. J. and Messing, G. L. (2006), Effect of Green Density on
the Thermomechanical Properties of a Ceramic During Sintering. Journal of
the American Ceramic Society, 89: 24482452. doi: 10.1111/j.15512916.2006.01097.x
Scott, G. D.; Kilgour, D. M.; (1969), The density of random close packing of spheres.
British Journal of Applied Physics, Series 2, Volume 2.
ftp://ftp.esc.cam.ac.uk/pub/gcs27/Backup_27_9_08/PhD/CSD/Scott%20&
%20Kilgour%201969.pdf
Sintering. (2015), Wikipedia.org. Wikimedia Foundation.
http://en.wikipedia.org/wiki/Sintering#Advantages.
Mueller 19

Sun, Yi-hua, Xiong, Wei-hao, and Li, Chen-hui. (2009), Fabrication of ultrahigh
density ZnO-Al2O3 ceramic composites by slip casting. Transactions of
Nonferrous Metals Society of China, 20(2010) 624-631
Aluminium Oxide. (2015), Wikipedia.org. Wikimedia Foundation.
http://en.wikipedia.org/wiki/Aluminium_oxide#Abrasive

MS Precision Balances.
http://us.mt.com/us/en/home/products/Laboratory_Weighing_Solutions/Precisi
on_Balances/MS_Precision_Balances.html
147 Digital Precision Calipers
http://www.generaltools.com/147--Digital-Fractional-Calipers_p_633.html

Mueller 20

Appendix A: Discussion of Data Analysis Methods

To determine the reproducibility of the results, a 95% confidence interval for
each value was calculated. The method used to determine the standard deviation
was the standard deviation function (stdev.s) in Microsoft Excel. This value was
multiplied by the student t-test value for 15 or 3 degrees of freedom, depending on
how many measurements were taken (16 or 4). These values are 1.753 and 2.353,
respectively. The product of this equation was then added and subtracted from the
mean, giving the upper and lower bounds, respectively.

Mueller 21

Appendix B: Experimental Data

Thickness (mm)

Pellet
#
1
2
3
4
5
6
7
8
Doubl
e
1
2
3
4
5

1.8
1
1.8
6
1.8
3
1.8
4
1.8
5
1.8
2
1.8
3
1.8
6
3.7
4
1.8
4
1.8
8
1.8
7
1.8
5
1.8

1.8

1.8
3
1.8
4
1.8
7
1.8
5
1.8
6
1.8
1
1.8
2
1.8

1.8
3
1.8
4
1.8
2
1.8
6
1.8
1
1.8

1.8
4
1.8
6
1.8
4
1.8
6
1.8
2
1.8

1.8
4
1.8

3.6
5
1.8
3
1.8
8
1.8
6
1.8
5
1.8

3.7

Mueller 22

1.8
5
1.8
2
1.8
7
1.8
3
1.8
1
1.8
1
1.8
3
3.6
8
1.8
6
1.8
4
1.8
6
1.8
2
1.8

1.8
2
1.8
9
1.8
8
1.8
4
1.8

Diameter
(mm)
me
an
1.82

Mass (g)

Green
Density
(g/cm3)

12.71

Powd
er
0.551

Pelle
t
0.531

2.297

1.85

12.74

0.553

0.533

2.260

1.84

12.75

0.55

0.524

2.235

1.86

12.69

0.552

0.529

2.254

1.83

12.74

0.549

0.525

2.246

1.81

12.73

0.550

0.521

2.264

1.8
2
1.8
6
3.7
3
1.8

1.82

12.74

0.550

0.526

2.262

1.83

12.77

0.552

0.524

2.236

3.70

12.8

1.099

1.062

2.231

1.83

12.76

0.553

0.521

2.226

1.8
8
1.8
7
1.8
7
1.8

1.87

12.79

0.556

0.550

2.284

1.87

12.78

0.550

0.541

2.258

1.85

12.79

0.550

0.533

2.247

1.83

12.77

0.551

0.537

2.286

3
6
1.7
9
7
1.8
9
8
1.7
5
Average
Value
Standard
Deviation
Upper
Bound
Lower
Bound

Temp
(C)
Pellet
#
1
2
3
4
5
6
7
8
Doubl
e
1
Mueller 23

3
1.8
3
1.8
3
1.7

3
1.8
4
1.8
5
1.7

4
1.8
6
1.8
9
1.7
1

4
1.8
7
1.8
8
1.6
9

1.84

12.79

0.551

0.530

2.244

1.87

12.82

0.551

0.530

2.198

1.71

12.78

0.549

0.490

2.234

1.83

12.759

0.551

0.528

2.252

0.04

0.0336

0.002

0.013

0.025

1.91

12.831

0.555

0.555

2.305

1.75

12.688

0.547

0.501

2.199

Time
(hrs)

Fired Thickness (mm)

1

mean

1400
1400
1400
1400
1400
1400
1400
1400
1400

0
0
0
0
0.1
0.1
0.1
0.1
0.1

1.63
1.61
1.57
1.59
1.52
1.53
1.57
1.53
3.05

1.58
1.62
1.6
1.61
1.53
1.54
1.56
1.53
3.06

1.57
1.6
1.58
1.6
1.52
1.54
1.55
1.54
3.06

1.59
1.61
1.57
1.6
1.52
1.54
1.54
1.54
3.06

1.61
1.61
1.56
1.59
1.55
1.55
1.54
1.54
3.07

1.60
1.61
1.58
1.60
1.53
1.54
1.55
1.54
3.06

1400

0.6

1.51

1.52

1.54

1.51

1.51

1.52

2
3
4
5
6
7
8

1400
1400
1400
1400
1400
1400
1400

0.6
0.6
0.6
1.2
1.2
1.2
1.2

1.61
1.58
1.56
1.56
1.54
1.57
1.46

1.65
1.58
1.54
1.55
1.56
1.56
1.44

Fired Diameter (mm)

Pellet
#
1
2
3
4
5
6

11.1
0
11.1
9
11.1
4
11.1
3
10.8
8
10.9
1

11.1
3
11.1
6
11.1
3
11.1
5
10.8
8
10.9
3

11.1
2
11.1
5
11.1
5
11.1
5
10.8
8
10.9
0

11.1
1
11.1
5
11.1
6
11.1
8
10.8
7
10.9
0

11.1
4
11.1
6
11.1
7
11.1
6
10.9
0
10.9
1

Mueller 24

mea
n
11.1
2
11.1
6
11.1
5
11.1
5
10.8
8
10.9
1

1.59
1.58
1.57
1.55
1.52
1.57
1.45

1.65
1.57
1.55
1.54
1.56
1.56
1.46

1.59
1.6
1.56
1.55
1.53
1.56
1.44

1.62
1.58
1.56
1.55
1.54
1.56
1.45

Fired Mass
(g)

Mass Loss
(g)

density
(g/cm3)

0.515

0.016

3.323

0.517

0.016

3.282

0.509

0.015

3.308

0.514

0.015

3.292

0.511

0.014

3.596

0.506

0.015

3.515

10.9
4
8
10.9
0
Doubl 10.7
e
0
1
10.7
1
2
10.6
9
3
10.7
0
4
10.7
0
5
10.6
7
6
10.6
5
7
10.6
6
8
10.6
4
Average
Value
Standard
Deviation
Upper Bound
Lower Bound

Mueller 25

10.9
0
10.8
9
10.7
0
10.7
2
10.7
0
10.7
0
10.7
1
10.6
6
10.6
9
10.6
7
10.6
7

10.8
9
10.8
9
10.6
9
10.7
4
10.7
2
10.7
1
10.7
1
10.6
7
10.7
1
10.6
8
10.6
8

10.9
0
10.9
0
10.6
7
10.7
6
10.7
2
10.7
5
10.7
2
10.6
9
10.7
2
10.7
5
10.6
8

10.9
3
10.9
0
10.6
5
10.7
7
10.7
4
10.7
9
10.7
2
10.7
1
10.7
3
10.7
5
10.6
8

10.9
1
10.9
0
10.6
8
10.7
4
10.7
1
10.7
3
10.7
1
10.6
8
10.7
0
10.7
0
10.6
7

0.511

0.015

3.521

0.510

0.014

3.561

1.031

0.031

3.760

0.506

0.015

3.679

0.534

0.016

3.661

0.525

0.016

3.670

0.517

0.016

3.687

0.521

0.016

3.752

0.515

0.015

3.714

0.515

0.015

3.661

0.474

0.016

3.656

0.513

0.015

3.555

0.012

0.001

0.165

0.539
0.486

0.017
0.014

3.906
3.204