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THE MANUFACTURING AND TESTING OF

INFUSION EPOXY RESIN CONTAINING


HAFNIUM CARBIDE MICRO-PARTICLES

Hamza Ebrahimji
[COMPANY NAME] [Company address]
INTRODUCTION
Epoxy resins have been around for a long time and have found quite a bit of use in our everyday lives
as adhesives and electrical and thermal insulators. These resins are usually mixed with hardeners to
produce solid polymers, which have a potential to be used for structural purposes. However, these
epoxy resins alone don’t usually posses the physical and mechanical properties necessary to be
considered viable as structurally sound materials. This is where addition of micro and Nano-particles
to the epoxy resin matrix is seen as a potential way of improving the aforementioned properties of
the resin. In this study we take a look at the manufacture and testing of infusion epoxy resin which
been modified by addition of Hafnium Carbide micro-particles.

AIMS
The aims of this project are to investigate the effect of adding Hafnium Carbide micro-particles into
infusion epoxy resin. The investigation hopes to determine the changes in mechanical properties of
epoxy resin by applying various tests in it.

OBJECTIVES
 To study the preparation and manufacture of infusion epoxy resin having numerous traces
of Hafnium Carbide.
 To investigate possible changes in mechanical properties of infusion epoxy resin upon
addition of microscopic particles of fillers.
 To investigate the changes that may occur in infusion epoxy resin using tensile test, 4-point
bending test, fracture toughness test and Barcol hardness test.
 To analyze the microstructure of the material using optical microscopy and SEM analysis.
 To identify the possible barriers to manufacturing of infusion epoxy resin with microscopic
particles of Hafnium Carbide.

LITERATURE REVIEW
Overview
Epoxy resin is a fairly useful polymer on its own. However sometimes the epoxy resin polymer on its
own does not meet the mechanical and chemical demands as effectively as desired. Hence addition
of various micro and nanoparticles into the polymer matrix is used to enhance the mechanical and
chemical properties of the epoxy resin polymer. We are trying to do the same by adding the Hafnium
Carbide micro particles into the infusion epoxy resin matrix. Others however, have done similar work
by adding compounds other than Hafnium Carbide into the epoxy resin matrix and testing the
mechanical and chemical properties of the resulting composite material. Here I try to detail some
these attempts and their outcomes.

Boron Carbide (B4C)


A study published in the Journal of Adhesion detailed the effect of boron carbide filler on the curing
and mechanical properties of an epoxy resin. The study made use of two different particle sizes and
amounts of reinforcing Boron Carbide that was filled into the matrix of the epoxy adhesive. Then the
gel time and degree of curing were measured followed by a study of the chemical structure of the
composite using Fourier Transform Infrared Spectroscopy (FTIR) and Boron Carbide distribution
analysis using Laser Confocal Microscopy. This was followed by the mechanical and thermal tests,
the Dynamic Mechanical Thermal Analysis (DMTA), to monitor viscoelastic properties and the glass
transition temperature (Tg) of the cured reinforced epoxy. The study then goes on to measure the
wear resistance of the reinforced epoxy against alumina using a pin-on-disc test, evaluated as a mass
loss. The wear tracks were studied by Scanning Electron Microscopy(SEM). To test the degree of
interaction between the Boron Carbide and the matrix, a bending strength test was carried out as
well. The results showed that the reinforced epoxy with Boron Carbide was very abrasive, wearing
the alumina. The reinforced epoxy had excellent mechanical properties that increased with Boron
Carbide content and with small particles. Moreover, the glass transition temperature value
decreased slightly upon Boron Carbide addition (J. Abenojar, 2009).

In another study published in The Journal of Adhesion Science and Technology, the effects of
moisture and temperature on an epoxy reinforced with Born Carbide, were studied. The specimens
were exposed to two moisture environments, 50 and 95% Relative Humidity (RH) at 60C to quantify
composite degradation level. Shore D hardness, three-point bending, and pin-on-disk wear tests
were used to determine the effect of humid environments. Mechanical properties were determined
at several exposure time intervals. Besides, the degradation process was analyzed with differential
scanning calorimetry (DSC) and infrared spectroscopy (FTIR–ATR). A general loss of properties was
observed after water absorption. However, most cases showed recovery after the drying process,
depending on the amount of water remaining in the material, which acts as a plasticizer, particularly
improving strength (J. Abenojar, 2012).

Titanium Dioxide (TiO2)


In a study published in the International Journal of Mining, Metallurgy and Engineering the
mechanical properties of micro and Nano Titanium Dioxide / epoxy composites were analyzed.
Epoxy with different volume fractions (1, 2, 3, 4, 5, 7, 10, 15 and 20 vol%) of microparticles TiO2 (50-
µm) and nanoparticles TiO2 (50-nm) were used to prepare epoxy micro composites and epoxy-
nanocomposites. The Nano-particles and micro-particles were dispersed into the resin system using
ultrasonic mixing process. By means of flexural testing, the mechanical performance of the
nanocomposites and micro composites was analyzed. Differential Scanning Calorimeter (DSC) was
used to evaluate the Glass Transition Temperature (Tg) and Scanning Electron Microscope (SEM)
techniques were used to examine the microstructure of the fracture surfaces in order to identify the
relevant fracture mechanisms involved.

The flexural strength and Young’s modulus of the Nano and micro-composites were found by means
of a three-point bending test. The results for the tests for Nano-composites is shown in Table 1.

From Table 1 it is evident that the flexural strength of the Titanium Dioxide/Epoxy Nano-composites
increase with increased volume fraction of nanoparticles with a maximum increment at 3% volume
fraction. This behavior can be attributed to decreasing space distance between cross-link chains
caused by “adding nanoparticles which are polar particles, creating van der- Waals bonding between
chains and particles leading to increase constrained between; particles/polymer chains and the
polymer chain itself” (L. Merad, 2011). Also from Table 1 it is obvious that the Young’s Modulus
increases with increase of filler addition due to particle agglomeration which leads to the increase in
constraint between polymer chains. For Titanium Dioxide/Epoxy Micro-particles, the results of the
three-point bending test can be seen in Table 2. It is evident from the table that the flexural strength
of Titanium Dioxide/Epoxy micro-composites decreases with increasing of the volume fraction of the
Titanium Dioxide microparticles. This can be attributed to low or missing interfacial strength
(adhesion. Debonding and cavitation appears because of particle size, shape and volume fraction. It
is also evident from the table that Young’s Modulus was increased by increasing the volume fraction
of Titanium Dioxide microparticles. This can be attributed to the size which lead to decrease in the
chains mobility (Ikram A. Al-Ajaj, 2013).The results of the thee point bending tests can be
summarized in the graphs on Figure 1 and Figure 2.

The glass transition temperatures of the samples were determined using the Differential Scanning
Calorimeter (DSC). The results obtained were put into the graph shown in Figure 3.

From graph in Figure 3 we can see that the glass transition temperature of EP/TiO2 Nano-composites
was increased at specific volume fraction while glass transition temperature decreased for other
TiO2 nanoparticles mixing ratios and for TiO2 microparticle additions. (Ikram A. Al-Ajaj, 2013)

After the specimen were fractured in the three-point bending test, the morphology of the fracture
surface was examined using Scanning Electron Microscope techniques. The following images (Figure
4, Figure 5 and Figure 6) of the surface features for neat epoxy of, EP/Nano 0% TiO2, EP/Nano 3%
TiO2 and EP/Nano 15% TiO2 were obtained.

From the images in Figure 4, Figure 5 and Figure 6, it was established that the nanocomposites with
minimum defects are the ones with low volume fractions of TiO2 nanoparticles. The morphologies of
the fractured surface shows that due to the presence of the TiO2 nanoparticles there exists brittle
fractures with dispersed stresses in more than one crack propagation direction and less flat area. It
was also noticed that the at around 4% vol. fraction of TiO2 nanoparticles the roughness of the
fractured structure was at a minimum value. (Ikram A. Al-Ajaj, 2013)

Silicon Dioxide (SiO2) and Aluminum Oxide (Al2O3)


This was a study carried out to assess the effect on the mechanical and thermal performance of
filling epoxy resins that were going to be used as insulators that support heavy conductors in
transmission systems. The epoxy resins act as a basic polymer matrix to which either Silicon Dioxide
micro and Nano-particles or Aluminum Oxide micro and Nano-particles are added. The study is
published in the journal Energy Procedia. The samples are prepared by planetary centrifugal mixing
techniques and degassed in a vacuum chamber to remove air bubbles before molding (Mu Liang,
2017). This process is summarised in Figure 7.

To actually test the mechanical properties of the prepared samples, Dynamic Mechanical Analysis
(DMA) is performed using the Perkin-Elmer DMA7e instrument in the tensile mode. The thermal
properties are tested using Thermal Gravimetric Analysis (TGA).

The Dynamic Mechanical Analysis was carried out by applying a small oscillating displacement to
obtain creep data. The samples are usually scanned over a range of temperatures. In this study the
Dynamic Mechanical Analysis was carried out at an oscillating frequency of 1 Hz, while the scanning
temperature was increased at a rate of 2°C/min from 40°C to 130°C. From the Dynamic Mechanical
Analysis, the storage modulus and loss modulus are measured from which the Tan delta and glass
transition temperature is obtained. These results are plotted into the graphs seen in Figure 8. The
Tan Delta results show that the nanocomposite samples exhibit a significant increase in glass
transition temperature compared to neat epoxy. An increase in glass transition temperature for 20%
micro Aluminum Oxide specimens (MC_A) is also noticed. However, a minimal increase in glass
transition temperature is noticed for both the Nano-micro-composite (NMC_A) and (NMC_S). When
it comes to the storage modulus the Aluminum Oxide filled nanocomposite (NC_A) has a higher
storage modulus before the glass transition temperature, from 30°C to 80°C, is reached. All the
micro-composite specimens show (MC_A and MC_S) show a high storage modulus after the glass
transition temperature, whereas the storage modulus of both the Aluminum Oxide and Silicon
Dioxide Nano-micro-composites (NMC_A) and (NMC_S) are similar to that of the neat epoxy prior to
the glass transition temperature, but a much lower storage modulus after the glass transition
temperature is observed for the Silicon dioxide filled specimen (NMC_S). these results can be seen
on the graphs in Figure 9. For the Loss modulus of the specimens a higher loss modulus is observed
for the two Aluminum Oxide filled nanocomposite and Nano-micro-composite (NC_A) and (NMC_A)
than the neat epoxy before the glass transition temperature. The micro-composite samples show a
large improvement in loss modulus after the glass transition temperature. The Silicon Dioxide filled
specimens are observed to have the same characteristics as that for the Aluminum Oxide filled
specimens. This is evident from the graphs in Figure 10.

Using the Perkin-Elmer TGA 7 thermal gravimetric analysis was performed. Using Nitrogen as the
filling gas, the test chamber temperature was increased from 30°C to 800°C at a heating rate of
10°C/min. The results were then plotted onto two separate graphs, one for Aluminum Oxide filled
specimens (Figure 11) and one for Silicon Dioxide filled specimens (Figure 12). For Aluminum Oxide
filled specimens the temperature of onset weight loss does not display any significant improvement
when compared to the neat epoxy. When compared to neat epoxy the rate of weight loss of micro-
composite and Nano-micro-composites is much lower. An improvement in the maximum weight loss
rate and the maximum weight loss temperature is observed for both the micro-composite and Nano-
micro-composite (NMC_S and NMC_A) specimens. The increased weight loss rate is however
correlated to the increased filler percentage loading.

The nanocomposites have a relatively larger onset weight loss rate and a similar maximum loss rate
compared with neat epoxy. The Silicon Dioxide filled specimen show fairly similar characteristics to
the Aluminum Oxide filled specimens, whereby the onset weight loss temperature is pretty much
the same but the onset weight loss rate is much smaller for micro-composite and Nano-micro-
composite. The silicon Dioxide nanocomposite’s characteristics are not different from those of the
neat epoxy. The maximum weight loss rate has a large improvement for micro-composite and Nano-
micro-composite (Mu Liang, 2017).

MATERIALS PROPERTIES AND APPLICATIONS


Infusion Epoxy Resins
Epoxy resins are basically polymers that contain at least two epoxide groups. The epoxide groups are
mostly an α-epoxy group which is situated terminally, cyclically or internally in a molecule which can
be converted to a solid through a thermosetting reaction (Goodman, 1998). Infusion epoxy resins
are resins that are formulated specifically for use as infusion matrices for production of composites.
The infusion epoxy resin that was being used is the SR 8100 from Sicomin. The resin itself has low
viscosity at ambient temperatures. The resin however, is not used on its own but is mixed with a
hardener SD 8824 and cured. The physical properties of SR 8100 alone can be seen in Table 3 and
the physical properties after hardener has been added and cured can be seen on Table 4 (Sicomin
Epoxy Systems, 2014). These infusion epoxy resins usually have a very good resistance to heat and
chemical attack especially from strong acids and alkali’s. therefore, these epoxy resins are very
useful as laminates for casting and the potting of electrical equipment. They are also very commonly
used as adhesives, especially for gluing metals (Raymond Aurelius Higgins, 2010).

Hafnium (IV) Carbide


Hafnium Carbide is a chemical compound of hafnium and carbon. Its appearance is that of a black
odorless powder which is usually obtained after the reduction of hafnium (IV) Oxide with carbon at
1800 to 2000°C It is mostly known as the most refractory binary compound known to man due to its
very high melting point of about 3900°C. It also quite dense with a density of 12.2 g/cm3 (Emeléus,
1968).The Hafnium carbide begins to oxidize at temperatures of about 430°C, which is fairly low
(Shimada, 1992). Hafnium Carbide is also extremely hard and corrosion resistant. This makes
Hafnium Carbide an excellent choice for use in high temperature applications such as jet engines,
rocket engines and high temperature ovens. Hafnium Carbide also has the ability to absorb slow
moving neutrons. This, together with its high refractory properties make it an ideal metal for the
manufacture of control rods for use in thermonuclear applications (Krebs, 2006).

MANUFACTURING PROCESS
The manufacturing process was done using the steps as detailed below:

First, the silicon mold was manufactured. A skeleton mold was made using a laser cutter from MDF
plastics, klerick plastic and wood. Then the volume of silicon rubber (SC25) needed to be poured in it
was calculated. Silicon was mixed with the hardener with a mixing ratio of 100:5, then was put into a
degassing chamber for 20 minutes to remove bubbles of air from it, after that it was poured into the
skeleton mold and left there for 2 days to be cured.

Secondly, the first batch of specimens was made using infusion epoxy resin(SR8100) with hardener
(SD8824) to get 5 specimens for 3 tests (tensile, 4-point bending and fracture toughness). First, a
releasing agent was put on the silicon rubber mold (CS25) to help get the specimen off the mold
without damaging it by brushing a small amount of it on the silicon. Then the mixing ratio was
calculated which came to about 100:22 between the hardener and the resin. After knowing how
much resin (107.8 g) and hardener (23.7 g) was needed, they were poured into a carton cup and
mixed using a wooden stick. After that my mix of hardener and resin was poured into the silicon
mold and left at room temperature for 24 hours for post curing, then put into the oven to gradually
increase the temperature form room temperature to 60°C for another 24 hours.

N.B: For the first batch that was done, a degassing chamber was used in the lab to remove all the air
bubbles form the mixture, but this was stopped because it had little effect, that was noticeable and
so a waste of time. This may have been due to the fact that an infusion epoxy resin was being used.

Thirdly, epoxy resin with Hafnium Carbide micro-particles was manufactured. First, calculations were
done to determine how much Hafnium was needed in the epoxy resin. 3% of Hafnium carbide was
put into epoxy resin and mixed manually. Then an ultra-sonic probe was used to make the micro-
particles get distributed uniformly into the resin. Then the mixture was poured into the silicon mold
and left for 24 hours at room temperature to post cure. After that it was put into the furnace for
another 24 hours and the temperature was elevated gradually until it reached 60°C.

The ultra-sonic probe used to disperse the microparticles into the epoxy matrix, did so by generating
ultra-sonic waves while it was immersed into the liquid suspension. The ultra-sonic waves cause
regions of alternating high pressure and low pressure to form in the liquid medium. This applies a
mechanical strain on the attracting electrostatic forces between the molecules of the epoxy resin
and causing some of them to break thus allowing the microparticles to fill in some of those spaces
creating a much more uniform agglomerate.
TESTING
Tensile test
Tensile tests are destructive tests that are carried out by taking a test-piece of known cross-sectional
area and placing it into a tensile-testing machine whose jaws grip the test piece at each end. The
machine then pulls apart the test-piece with increased increments of tensile force. The machine
then measures the amount of force being experienced by the test-piece using a load cell. Then for
each increment of force the amount by which the length of a known ‘gauge length’ on the test-piece
increases is measured (Higgins, 2006). From the tensile test we obtain a graph of force against
extension or a graph of Stress vs Strain as seen on Figure 23. From this graph the following values for
the material can be obtained:

 Ultimate Tensile Strength


 Yield Strength
 Fracture Stress or Breaking Stress
 Offset Strain (typically 0.2%)

From the same graph we can also obtain the Young’s Modulus of the material as well. We know that
the Youngs Modulus, E, of a material is given by:
𝜎
𝐸=
𝜀
Equation 1:Young's Modulus

Where: 𝜎= Tensile Stress (MPa)

𝜀 =Tensile Strain (mm)

Therefore, from the graph the Young’s Modulus of the specimens is collected by finding the gradient
of the straight part of the graph.

The specimens were first measured out as shown in Figure 24, and the dimensions obtained were as
follows:

 Initial gauge length = 90 mm


 Speed = 1 mm/s
 Thickness= 4 mm

The Specimens were placed into the tensile testing machine one by one and the load and extension
data was produced. From this the Tensile Stress and Tensile Strain of the specimens were calculated
and the graphs of Stress against Strain were plotted using Microsoft Excel. The resultant graphs for
the specimens with Hafnium Carbide and the ones without can be seen on Graph 1 and Graph 2
respectively.

From Graph 2, the following results were obtained for specimens without any infused Hafnium
Carbide:

1) Epoxy 1:
 Young’s Modulus = 1233.8 MPa
 Ultimate Tensile Strength = 31.12 MPa
 Yield Stress = 20.0 MPa
 Fracture Stress = 22.44 MPa

2) Epoxy 2
 Young’s Modulus = 1292.0 MPa
 Ultimate Tensile Strength = 46.62 MPa
 Yield Stress = 31.0 MPa
 Fracture Stress = 25.50 MPa

3) Epoxy 3
 Young’s Modulus = 1271.0 MPa
 Ultimate Tensile Strength = 24.12 MPa
 Yield Stress = 18.0 MPa
 Fracture Stress = 13.89 MPa

4) Epoxy 3 retest
 Young’s Modulus = 1193.40 MPa
 Ultimate Tensile Strength = 40.71 MPa
 Yield Stress = 21.50 MPa
 Fracture Stress = 40.33 MPa

5) Epoxy 3 retest 2
 Young’s Modulus = 1069.2 MPa
 Ultimate Tensile Strength = 11.26 MPa
 Yield Stress = 9.50 MPa
 Fracture Stress = 6.43 MPa

6) Epoxy 3 slipped
 Young’s Modulus = 1234.10 MPa
 Ultimate Tensile Strength = 41.56 MPa
 Yield Stress = 20.70 MPa
 Fracture Stress = 23.28 MPa

7) Epoxy 3 slipped again


 Young’s Modulus = 1325.4 MPa
 Ultimate Tensile Strength = 38.02 MPa
 Yield Stress = 15.10 MPa
 Fracture Stress = 11.45 MPa

8) Epoxy 4
 Young’s Modulus = 1321.5 MPa
 Ultimate Tensile Strength = 44.48 MPa
 Yield Stress = 22.10 MPa
 Fracture Stress = 23.99 MPa

9) Epoxy 4 slipped
 Young’s Modulus = 1321.5 MPa
 Ultimate Tensile Strength = 41.30 MPa
 Yield Stress = 23.0 MPa
 Fracture Stress = 21.83 MPa
10) Epoxy 5
 Young’s Modulus = 1028.60 MPa
 Ultimate Tensile Strength = 40.31 MPa
 Yield Stress = 22.0 MPa
 Fracture Stress = 22.20 MPa

And from Graph 1, the following results were obtained for the specimen infused with Hafnium
Carbide.

11) HFC 1
 Young’s Modulus =1306.7 MPa
 Ultimate Tensile Strength = 48.24 MPa
 Yield Stress = 22.0 MPa
 Fracture Stress = 27.93 MPa

12) HFC 2 Slipped


 Young’s Modulus =1221.3 MPa
 Ultimate Tensile Strength = 34.05 MPa
 Yield Stress = 17.50 MPa
 Fracture Stress = 28.68 MPa

13) HFC 5
 Young’s Modulus =1296.2 MPa
 Ultimate Tensile Strength = 48.53 MPa
 Yield Stress = 24.0 MPa
 Fracture Stress = 27.86 MPa

14) HFC 2 Retest


 Young’s Modulus = 1124 MPa
 Ultimate Tensile Strength = 18.72 MPa
 Yield Stress = 12.75 MPa
 Fracture Stress = 10.21 MPa

15) HFC 3
 Young’s Modulus = 1279.2 MPa
 Ultimate Tensile Strength = 46.29 MPa
 Yield Stress = 22.0 MPa
 Fracture Stress = 27.33 MPa

16) HFC 4 Retest


 Young’s Modulus = 1401.9 MPa
 Ultimate Tensile Strength = 39.98 MPa
 Yield Stress =18.9 MPa
 Fracture Stress = 21.42 MPa
17) HFC 4 Slipped
 Young’s Modulus =1382.7 MPa
 Ultimate Tensile Strength = 40.68 MPa
 Yield Stress = 17.0 MPa
 Fracture Stress = 20.07 MPa

Fracture Toughness
“Fracture is a form of failure that is defined by the separation or fragmentation of a solid body into
two or more parts under the action of stress.” (Kailas, 2011). Fracture toughness is representation of
the amount of stress required to propagate a preexisting flaw. A flaw can be a crack, void,
metallurgical inclusions, weld defects or design discontinuities (NDT Resource Centre, 2012).
Fracture toughness testing is carried out by first creating a sample like the one in Figure 25. The
dimensions of the sample are taken, including the crack width. Then this sample is placed in a
Universal Testing Machine which will apply an incrementally increasing load on the sample and
measure its extension until failure occurs.

Specimen Dimensions:

 Crack Length, a = 16.00mm


 Specimen Width, W= 32.00mm
 Specimen Thickness, B= 5.00 mm

From the load and extension data collected, load vs extension graphs were drawn for all the
specimens. From these graphs, Pq was determined by using a 5% off-set line. From the, B, W and a of
the specimen we can determine:
𝑎 𝑎 𝑎 𝑎 𝑎
𝑎 (2 + ) {0.886 + 4.64 − 13.31( )2 + 14.72( )3 − 5.6( )4 }
𝑓( ) = 𝑊 𝑊 𝑊 𝑊 𝑊
𝑊 𝑎 3
(1 − 𝑊 )2

Equation 2: Formula for f a/W

Substituting the values of a and W into Equation 2, we get the value of f a/W:
𝑎
𝑓 ( ) = 119.312
𝑊
From this we can calculate Kq, from the formula:
𝑃𝑞 𝑎
𝐾𝑞 = × 𝑓( )
𝐵 × √𝑊 𝑊
Equation 3: Formula for Kq

We then check the validity of our sample by:


𝐾𝑞
𝐵, 𝑎 ≥ 2.5 × ( )2
𝜎𝑦
Equation 4: Validity check for fracture toughness sample

If the sample is valid then Kq = KIC.


The data collected from the fracture toughness test is plotted onto the load vs extension graphs
shown in Graph 3 and Graph 4.

From Graph 3 the following values for Pq for each specimen with HfC are derived and the value of Kq
is calculated:

1) Epoxy + HfC run 1


 Pq = 294.27 N
 Kq = 39.25 MPa.m1/2

2) Epoxy + HfC run 2


 Pq =283.08 N
 Kq = 37.76 MPa.m1/2

3) Epoxy + HfC run 3


 Pq = 158.15 N
 Kq = 21.10 MPa.m1/2

4) Epoxy + HfC run 4


 Pq =278.16 N
 Kq = 37.10 MPa.m1/2

5) Epoxy + HfC run 5


 Pq = 220.27 N
 Kq = 29.38 MPa.m1/2

From Graph 4 the values of Pq is determined for the specimens without HfC and the values of Kq are
calculated:

6) Epoxy Run 1
 Pq = 358.86 N
 Kq = 47.87 MPa.m1/2

7) Epoxy Run 2
 Pq = 438.40 N
 Kq = 58.48 MPa.m1/2

8) Epoxy Run 3
 Pq = 287.28 N
 Kq = 38.32 MPa.m1/2

9) Epoxy Run 4
 Pq = 343.99 N
 Kq = 45.89 MPa.m1/2

4-point Bending:
Bend tests are often used as a means of judging the suitability of a metal for similar treatment
during a production process. the four-point bending test, as the name suggests, is used to test the
beam of a known cross-section by applying a load on it at four points, two at the ends of the beam
from the bottom and two at the near the center of the beam at the top. This is usually carried out by
a specific test fixture on the universal testing machine. The beam is loaded at a constant rate until
failure occurs. However, before the beam is loaded, its dimensions and the dimensions of the testing
apparatus are taken.

The four-bending flexural test provides values for the modulus of elasticity in bending, Ef, flexural
stress σf and flexural strain, εf (Harvey, 2012). The universal testing machine produces the load and
extension data, from which the flexural stress and strain is calculated.

Specimens dimensions:

Length = 80 mm, width = 10 mm, thickness= 4 mm

During test:

Outer span= 66 mm

Inner span= 22 mm

Length= 80 mm

Width = 10 mm

The results of the 4-point bending test are plotted on Graph 5 and Graph 6. From Graph 6, using the
linear portion of the stress strain curve, the flexural Young’s Modulus was calculated:

1) Epoxy + HfC run 1


 Ef = 3526.5 MPa

2) Epoxy + HfC run 2


 Ef = 4884.3 MPa

3) Epoxy + HfC run 3


 Ef = 4611.0 MPa

4) Epoxy + HfC run 4


 Ef = 3074.4 MPa

5) Epoxy + HfC run 5


 Ef = 3474.8 MPa

From Graph 6 the values of the flexural Young’s Modulus was calculated for the specimens without
HfC:

6) Epoxy Run 1
 Ef = 4911.7 MPa

7) Epoxy Run 2
 Ef = 2779.1 MPa

8) Epoxy Run 3
 Ef = 5228.0 MPa

9) Epoxy Run 4
 Ef = 3939.2 MPa

10) Epoxy Run 5


 Ef = 5089.5 MPa
Barcol Hardness test
The Barcol Hardness Test is a method to check the indentation hardness of a material through the
depth penetration of an indentor loaded on a material sample. This penetration depth of the
indentor is then compared to the penetration of a reference material (Lawrence C. Bank, 2003).This
method is very suitable to measure the hardness of softer materials such as reinforced thermoset
resins. It can also be used to determine the degree to which a resin has cured. The Barcol Hardness
test is performed using the Barcol Impresser, which can be seen in Figure 28. Its operation involves
the tip being pressed against the material. The depth of the tips indentation, which depends on the
hardness of the material, is transferred by a tension spring and lever to be read on the dial (Bennett,
1967). After the test was performed on the samples, the following results were obtained:

 With HfC= roughly 29 Barcol Hardness


 Without HfC = roughly 29 Barcol Hardness

DISCUSSION OF RESULTS OBTAINED


From the tensile tests it was observed that the mean Young’s Modulus for specimen without HfC is
1229.05 MPa whereas the mean Young’s Modulus for specimens with HfC is 1287.43 MPa.
Therefore, it is obvious that adding the HfC into the epoxy resin improves its Young’s modulus. From
the stress vs strain graphs (Graph 1 and Graph 2) it is evident that the samples of both specimens,
with or without HfC did not undergo a lot of necking before fracture. However, both the mean
Ultimate Tensile Strength and the mean Fracture Strength for specimens with HfC,39.50 MPa and
23.07 MPa respectively, is more than that of specimens without, 35.95 MPa and 21.13 MPa
respectively. With these results it can be said that adding the HfC to the epoxy resin does improve its
overall strength, although not by much. This increase in strength with addition of microparticles
could be attributed to the reduction of chain-mobility of the polymer matrix due to the size of the
added microparticles.

From the Fracture toughness test, we can see that the mean working fracture toughness for
specimens with HfC is lower, at 32.92 MPa.m1/2, than that for specimens without HfC, at 47.64
MPa.m1/2.This can be attributed to the agglomeration of the microparticles causing a reduction in
elasticity in the entire matrix. From these mean working fracture toughness we also see that none of
the values are valid.

From the 4-point bending test it was again observed that the mean flexural Young’s Modulus for
specimens with HfC was 3914.2 MPa while that for specimens without of HfC was 4389.5 MPa.
Although this might seem counter-intuitive at first it is actually what is expected. With addition of
micro-particles, the interfacial strength is lowered between the molecules due to adhesion,
debonding and cavitation because of the varying particle sizes.
MICROSCOPY

Post Microscopy Preparation

First of all, two specimens of each batch (with and without HfC) were chosen and the epoxy resin
poured on them to manufacturer a carrier. The epoxy carrier then was grinded to be stable from
each side. The tip of the specimen was grinded in 3 stages (220 paper, 400 and finally 600) after
grinding we polished the tip of the specimens using the same machine first with spraying 6 micron
on the 6-micron circular plate on a rotating speed of 300 then 1 micron spraying with 1-micron plate
with a rotating speed of 400.

1. Optical Microstructure
Using an Optical Microscope, images were taken of the prepared samples of both specimens
with HfC and without HfC. The images were taken at various magnifications, starting from 5x
magnification to 100x magnification as seen on Figures 32 to 41.

i. 5x Magnification
At the 5x magnification level there is no visible difference between the specimens with HfC and
those without HfC.

ii. 10x Magnification


At the 10x magnification level there is a more noticeable difference between the two specimens.
The specimen with HfC can be seen having more visible black spots on the surface than the
specimen without HfC. These black spots can be assumed to be the HfC microparticles that have
agglomerated into the resin matrix.

iii. 20x Magnification


Here together with more black spots, it was also noticed that the linear streaks on the specimen
with HfC are more unidirectional than those on the specimens without HfC, implying a more regular
crystalline structure.

iv. 50x magnification


The specimen with HfC, was noticed to have more linear streaks compared to the specimens
without. This could imply that the more regular structuring could be a result of the added HfC
microparticles into the epoxy resin matrix.

v. 100x Magnification
For the specimen with HfC, at this magnification it was very clearly observed that the structure
looked more homogeneous, with smaller grain sizes and no voids. This is evidence of the proper
agglomeration of the HfC into the epoxy resin matrix by the ultra-sonic probe. It is also evidence of a
more crystalline structure that the composite displays compared to the amorphous structure of the
original epoxy resin.

2. Confocal microscopy
The Confocal microscope makes use of an arrangement of diaphragms which act as appoint
of the source and as a point of the detector at optically conjugate points on the path of the
rays. This allows the rays which are out of focus to be suppressed by the detection pin hole.
To obtain the full image, the image point is moved across the specimen by mirror scanners.
A photomultiplier converts the reflected light passing through the detector pinhole into
electrical signals which are used to recreate the image on a computer display. The confocal
laser microscope that was used can be seen in Figure 29.

From the Confocal Micrographs in Figure 42 and 43 it is obvious that the roughness results
obtained decrease after adding the HfC micro-particles to the epoxy resin matrix. This can be
attributed to the micro-particle agglomeration into the matrix causing the overall structure
to be more crystalline than before.

3. Scanning Electron Microscopy

Scanning electron microscopy makes use of a scanning electron microscope to take detailed images
at extremely high magnification levels. Unlike a regular microscope, the SEM makes use of electrons
which bombard the sample, and the reflected electrons are captured by special sensor to create an
image.

Before a sample can be put into the SEM, it has to be thoroughly cleaned of all grease, moisture and
dust to avoid any outgassing from organic contamination and water. This was done by using a
volatile solvent like acetone, which can be then dried off easily by compressed gas (Zhang, 2008).

Carbon coating is important because the specimen is not conductive, so we need to make it
conductive, so it could be used in SEM MICROSCOPY.

 First the carbon nodes were prepared.


 Sticking the specimen to the cylindrical using double sided carbon tape.
 Paint the side of the specimens with silver paint
 Place the carbon node into the upper chromium compartment.
 Put the specimen inside the chamber to start the carbon coating
 Do it twice because we want double layers

The results for the SEM can be seen in the Appendix (V). From these results we can conclude that
the SEM microscopy was successful, because it shows that the HfC particles was shown to be
distributed uniformly across the epoxy this shows that ultra-sonic probe was successful, and it was
able to distribute the particles. We even went to 1000 micro-meters magnification and it the
particles were also approximately 3% as excepted.

CONCLUSION
In conclusion we can say that the addition of HfC into the polymer matrix of the epoxy resin is fairly
easy to perform especially with an ultra-sonic probe. The properties of the micro composite were
also observed to have improved slightly when it came to lateral loading. However, the for loads
applied longitudinally, the micro-composite was actually out performed by the neat epoxy resin. This
could be attributed to the more regular structure, closer to crystalline structure of the micro-
composite as compared to the more irregular and amorphous structure of the neat epoxy resin as
was seen in the optical micrographs.
This study, however was limited to only using 3% volume fraction of HfC microparticles to make the
micro-composite. Further studies can be performed where the properties of micro-composites with
different volume fractions can be manufactured and tested.

REFERENCES
Bennett, R. B., 1967. Impressor Impresses Industry. Barber-Colman News, September.

Emeléus, H. J., 1968. Hafnium. In: Advances in Inorganic Chemistry and Radiochemistry. s.l.:Academic
Press, pp. 169-170.

Goodman, S. H., 1998. Epoxy Resins. In: Handbook of Thermoset Plastics (Second Edition). 2nd ed.
s.l.:William Andrew Applied Science Publishers, pp. 193-268.

Harvey, P. &., 2012. Four Point Bending. s.l.:Taylor & Francis Group.

Higgins, R. A., 2006. Mechanical Testing. In: Materials for Engineers and Technicians. s.l.:Newnes.

Ikram A. Al-Ajaj, M. M. A. a. H. I. J., 2013. Mechanical Properties of Micro and Nano TiO2/Epoxy
Composites. International Journal of Mining, Metallurgy & Mechanical Engineering , 1(2), pp. 93-97.

J. Abenojar, M. A. M. ,. F. V. ,. V. P.-S. &. J. M. M.-M., 2009. Effect of Boron Carbide Filler on the
Curing and Mechanical Properties of an Epoxy Resin. The Journal of Adhesion , 85(4-5), pp. 216-238.

J. Abenojar, M. A. M. F. V. &. J. C. d. R., 2012. Effect of Moisture and Temperature on the Mechanical
Properties of an Epoxy Reinforced with Boron Carbide. Journal of Adhesion Science and Technology,
25(18), pp. 2445-2460.

Jeelani, R. M. R. H. M. V. K. R. N. C. S., 2005. Infusion of SiC Nanoparticles Into SC‐15 Epoxy: An


Investigation of Thermal and Mechanical Response. Macromolecular Materials and Engineering,
290(5), pp. 423-429.

Kailas, P. S. V., 2011. Failure . In: Material Science . Bangalore: Indian Institute of Science.

Krebs, R. E., 2006. Hafnium. In: The History and Use of Our Earth's Chemical Elements: A Reference
Guide. s.l.:Greenwood Publishing Group, p. 150.

L. Merad, B. B. M. J. A. A. a. J. P. C., 2011. Characterization and Mechanical properties of Epoxy Resin


Reinforced with TiO2 nanoparticles. Journal of Engineering and Applied Sciences, Volume 6, pp. 205-
209.

Lawrence C. Bank, T. R. G. ,. B. P. T. ,. J. S. R., 2003. A model specification for FRP composites for civil
engineering structures. Construction and Building Materials, Volume 17, pp. 405-437.

Mu Liang, K. L. W., 2017. Study of mechanical and thermal performances of epoxy resin filled with
micro particles and nanoparticles. Energy Procedia , Volume 110, pp. 156-161.

NDT Resource Centre, 2012. Fracture Toughness. [Online]


Available at: https://www.nde-
ed.org/EducationResources/CommunityCollege/Materials/Mechanical/FractureToughness.htm
Raymond Aurelius Higgins, W. B., 2010. Materials for Engineers and Technicians. s.l.:Routledge.

Shimada, S., 1992. Oxidation Kinetics of Hafnium Carbide in the Temperature Range of 480 to 600C.
Journal of the American Ceramic Society, 75(10), pp. 2671-2678.

Sicomin Epoxy Systems, 2014. SR 8100 Epoxy system for Injection and Infusion. s.l.:Sicomin.

Zeng, G. J. H. Z. C. Q. M., 2009. Mechanism of interactions of eggshell microparticles with epoxy


resins. Polymer Engineering and Science, 49(7), pp. 1383-1389.

Zhang, H., 2008. SEM Sample Preparation instructions, s.l.: s.n.


APPENDIX
I. Calculation:

Calculation 1: Volume of Silicon Rubber Required


Calculation 2: Volume of Silicon Rubber Required Continued
Calculation 3: Epoxy and Hardener Mass Required Calculation
Calculation 4:Hafnium Carbide Required
II. Figures:

Figure
1:Varaition
of Flexural
Strength of
TiO2 volume
fraction of
EP/TiO2
Nano-
composite
and EP/TiO2
micro-
composite

Figure 2: Youngs Modulus versus TiO2 Volume fraction of EP/TiO2 Nano-composites and EP/TiO2 Micro-composites
Figure 3: Glass transition temperature of epoxy, EP/TiO2 micro-composites and EP/TiO2 Nano-composites (Ikram A. Al-Ajaj,
2013)
Figure 4: Topography of Fractured Surface of EP/Nano 0% TiO2 Figure 5: Topography of Fractured Surface of EP/Nano 3%
TiO2

Figure 6: Topography of Fractured Surface of EP/Nano 15% TiO2

Figure 7:Sample preparation procedure for epoxy resin filled with SiO2 or Al2O3 (Mu Liang, 2017)
Figure 8: (left)Tan Delta of Al2O3 filled specimens;(right) Tan Delta of SiO2 filled specimen (Mu Liang, 2017)

Figure 9:(left) Storage Modulus for Al2O3 filled specimens;(right) Storage Modulus SiO2 filled specimens
Figure 10: (left) Loss Modulus of Al2O3 filled specimens;(right) Loss Modulus of SiO2 filled specimen

Figure 11:Thermal Gravimetric Analysis results for Al2O3 filled specimens (Mu Liang, 2017)
Figure 12: Thermal Gravimetric Analysis results for SiO2 filled specimens (Mu Liang, 2017)
Figure 13:Skeleton Mold for Silicon Rubber 1

Figure 14:Skeleton Mold for Silicon Rubber 2


Figure 16: Silicon Rubber Mold 2

Figure 15:Silicon Rubber Mold 1


Figure 18: Epoxy Hardener Figure 17: Infusion Epoxy Resin

Figure 19: Epoxy Resin Specimens


Figure 21: Hafnium (IV) Carbide Figure 20:Ultra-Sonic Probe

Figure 22: Epoxy +3% HfC Specimens


Figure 23: Stress Strain CurveInvalid source specified.

Figure 24 Tensile test dimensions


Figure 27: Specimen Dimensions for Fracture Toughness test

Figure 25: Specimens of Epoxy only after testing Figure 26: Specimens with HfC after testing
Figure 28: Bracol Hardness Equipment
Figure 30:Monocrystalline Diamond Solution
Figure 31: Polycrystalline Diamond Solution

Figure 29:Laser Confocal Microscope


Figure 35: 5x micrograph without HfC
Figure 37: 5x micrograph with HfC

Figure 34:10x micrograph without HfC


Figure 36:10x micrograph with HfC

Figure 33:20x micrograph with HfC Figure 32:20x micrograph without HfC
Figure 41:50x micrograph with HfC
Figure 40: 50x micrograph without HfC

Figure 39: 100x micrograph with HfC


Figure 38:100x micrograph without HfC
Figure 42: Confocal micrograph of specimen before addition of HfC
Figure 43: Confocal micrograph after addition of HfC
III. Tables:

Table 1: Compositions and Mechanical Properties of TiO2/Epoxy Nano-composites (Ikram A. Al-Ajaj, 2013)
Table 2: The Compositions and Mechanical properties of TiO2/Epoxy Micro-composites (Ikram A. Al-Ajaj, 2013)
Table 4:Epoxy Resin SR8100 Physical Properties

Table 3:SR 8100 /SD 882x Mix Physical Properties


IV. Graphs

Stress vs Strain Graph For Epoxy with HfC


55

50

45

40

35

30
Tensile Stress (MPa

HFC 1
HFC 2 slipped
25 HfC 5
HfC 2 retest
20 HfC 3
HfC 4 retest
15 HfC 4 slipped

10

0
0 0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04 0.045 0.05 0.055 0.06 0.065 0.07 0.075 0.08 0.085 0.09 0.095

-5
Tensile Strain (mm)

Graph 1: Stress vs Strain Graph for Specimens with HfC


Stress vs Strain For Epoxy Only
50

40
Epoxy 1

Epoxy 2

Epoxy 3
30

Epoxy 3 retest
Tensile Stress (MPa)

Epoxy 3 retest
2
20
Epoxy 3
slipped
Epoxy 3
slipped again
Epoxy 4
10

Epoxy 4
slipped
Epoxy 5

0
0 0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04 0.045 0.05 0.055 0.06 0.065 0.07 0.075 0.08

-10
Tensile Strain (mm)

Graph 2: Stress vs Strain for Specimens without HfC


Load vs Extension For Specimen with HfC

350

300

250

200
HFC 1
HFC 2
Load (N)

HFC 3
150
HFC 4
HFC 5

100

50

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2 1.3 1.4

-50
Extension (mm)

Graph 3: Load vs Extension for Fracture Toughness for Specimens with HFC
Load vs Extension For Specimens without HfC

500

450

400

350

300

Epoxy 1
250 Epoxy 2
Load (N)

Epoxy 3
200 Epoxy 4

150

100

50

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2 1.3 1.4

-50
Extension (mm)

Graph 4: Load vs Extension for Fracture Toughness analysis for Specimens Without HFC
Flexural Stress vs Flexural Strain for Specimens with HfC

165
160
155
150
145
140
135
130
125
120
115
110
105
100
95
Flexural Stress (MPa)

90
85
80
75 Epoxy + HfC 1
70
65 Epoxy + HfC 2
60
55
50 Epoxy + HfC 3
45
40
35 Epoxy + HfC 4
30
25
Epoxy + HfC 5
20
15
10
5
0
-5 0 0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04 0.045 0.05 0.055 0.06 0.065 0.07 0.075 0.08 0.085 0.09
-10
Flexural Strain (mm)

Graph 5: Flexural stress vs Flexural strain for specimens with HfC


Flexural Stress vs Flexural Strain for Epoxy without HfC

180

170

160

150

140

130

120

110

100 Epoxy 1
Flexural Stress

Epoxy 2
90
Epoxy 3
80
Epoxy 4
70
Epoxy 5
60

50

40

30

20

10

0
0 0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04 0.045 0.05 0.055 0.06 0.065 0.07
-10
Flexural Strain

Graph 6:Flexural stress vs Flexural strain for Specimens without HfC


V. Scanning Electron Microscopy
Settings

Phases for Acquisition


Phase Fraction

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