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Carbon Composite Imaging and Analysis

Composite materials are materials of which physically combine two or more materials of

different properties into one material that we create to have different properties than each

individual material on its own. [1] A carbon composite material is a material that is combined

with a polymer to have properties differing from just carbon fiber and just polymers on their

own. [2] This mixture contains carbon fibers within a polymer resin. This type of material can be

referred to a carbon-fiber reinforced plastic. The possible binding polymers can vary according

to what you need the material to perform. These different binding polymers include polyester,

vinyl ester, or even nylon. You can also add in different fiber materials with the carbon fibers,

even other polymers or to strengthen and adjust the material properties. There are also carbon

nanotube enforced polymers, which use carbon nanotubes in addition to carbon fibers in the

composite. These can be referred to as graphite-reinforced polymers, and typically have

properties of being tougher and stronger than carbon fiber reinforced polymers.

Carbon composite materials have a wide range of applications due to their lightweight and

strong properties. The most important takeaway to make up for the cost of making these

materials is their ‘strength-to-weight ratio’. These materials are used in supercars for racing,

mainly due to their lightweight properties allowing the vehicles to get up to top speed with

strength and without holding the car back with much weight. This even allows the cars to be

smaller, and more aerodynamic. They are also used for reinforcing bridges and other old

structures through the process of retrofitting. Adding the polymer to a carbon material allows the

materials to not be as brittle, but still keep its strength, this allows applications to reinforce

concrete structures and improving their shear and tensile strengths. These materials are

preferable, but more expensive than steel. An application of carbon nanotube reinforced

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polymers is in mountain bike tires. These tires use carbon nanotubes for strength and durability.

A surprising application of this material is in fabrication and use as microelectrodes. They take

the carbon nanotubes and epoxy-seal them into a glass capillary for use as a microelectrode. As

we learn more about and create a widening range of these materials, more applications in every

field of design and stem occur.

There are a few different ways to fabricate carbon composite materials. The sample I

analyzed was made by the ‘sandwich’ method. This isn’t necessarily a technical term, but each

layer of the carbon came pre-woven. A student at the University of Utah composite materials lab

created them by taking one layer, applying an epoxy layer, then placing another layer of the

carbon fibers ninety degrees to the first layer, and so on. She came to me with the problem of

worrying the carbon fiber layers had come with inconsistencies. As she analyzed the carbon fiber

material, she realized it did not lay flat. She of course first checked her method of fabrication,

where she reassured that she had laid the layers out correctly, and that it was not due to user error

that the material was warped. She sent her materials to me to image with the SEM we have to

measure the layers for her. She had previously analyzed the samples with an optical microscope.

She sent me with samples she cut off of the edge of the material, each about 5 mm by 4 mm by

varying lengths to image. I took images on the top and either side of each of the four samples she

provided. When she handed over the samples, she explain that as you looked at the side of the

composite piece, I would see alternating layers coming at me and going across the screen.

The first image I obtained was a completely-covered-with-epoxy side (Figure 1), which was

discouraging, as I expected to see carbon fibers, and I couldn’t quite figure out why I wasn’t

seeing carbon fibers until I became a little more familiar with the samples, and realized it was the

epoxy side of the composite. This side would be a layer of all epoxy resin that helps keep

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everything together. As I imaged more samples, I eventually got some pretty good images of the

carbon fibers going across the screen; this showed confirmation of fiber orientation (Figure 2).

When she gave me the samples, she mentioned she attempted to sand and polish the edge of the

samples so I could measure the width of each layer more accurately, but as you can see in Figure

3, the sanding was slightly misleading in that it made it hard to identify the layers, because the

scratched on the composite were visible in my image.

I must mention was that in Figures 3 and 4, I saw charging. I would have set the SEM to

charge up reduction mode, but I did not want to sacrifice the contrast in the image, since it was

already difficult to see the fibers and identify the layers. Since there was charging, I did an

elemental analysis using the x-ray machines with the SEM to identify what was causing the

charging (Figures 5 through 8). Once I did this, I was inclined to believe that the charging was

occurring due to the polymer layers of the composite material. This is because most of the sulfur

was placed at the location of charging. Due to the sample containing sulfur and oxygen, and

since I was not told which type of polymer was used to link the carbon fiber sheets together, and

after using the quantification of the elements in the sample at that image location, I determined

that the polymer they used may have been polyphenylene sulfide. [3][4] Polyphenylene sulfide is a

commonly used polymer for composite materials. Since this ‘engineering plastic’ consists of a

benzene ring with a sulfur group attached to it (Figure 9) , and since the oxygen seemed to be

pretty readily dispersed over the entire image, this conclusion seems to be quite sound.

Polyphenylene sulfide is considered to be a useful high-performance thermoplastic of which can

be used and worked with at high tolerance to molding, extruding, and machining. Its high

resistance to a wide range of environments is desirable for all applications as a fiber.

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One of the most important reasons I was imaging these samples for the University of Utah

student, was to measure the layers of carbon to obtain information as to whether or not the actual

layers were at fault for the warping of the composite as a whole. I made measurements at

different parts of each sample she gave me, and different magnifications just to make sure

(Figures 10 through 12). Each measurement of width seemed approximately the same, give or

take a few micrometers. In figure 12, you can see that the middle layer of carbon fibers that is

coming out at you is significantly larger than the immediately lower layer that is coming toward

you, three times as bigger to be approximate. The middle layer measures in at 396 µm, while the

lower layer measures in at 135 µm. This may be because the layers may have been mixed up, or

a varying thickness for strength. Also, there is a slight visible difference in the width of the

middle layers as you look across it. The measurements indicate this difference is approximately

10 µm difference, so this little of a difference should not have caused the warping she was

experiencing.

Fracturing[5] in carbon composites is less common than in carbon fibers themselves, due to

the decrease in brittleness of the material while combing with a polymer that is less brittle. As we

continue to use these materials, we need to understand and analyze different method of failure.

This failure in my image of that area of the sample (Figure 13) seemed to be due to a puncture or

tensile strain on the material, causing the breakage of several carbon fibers. Carbon and its

composites tend to have a relatively high level of brittleness, this is why I am hesitant to use

completely carbon fiber rims for my mountain bike. The impact and compression/tension forces I

would be applying while riding downhill, would cause possible crack propagation and complete

failure of my rim, and that’s dangerous. Enve rims[6] is a composites company based in Ogden,

Utah that makes bike parts using composites, including carbon fiber reinforced polymer

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composites. There is a rim on display at the Leonardo in Salt Lake City displaying how light a

rim of theirs is, and weight means a lot when you are a racer, especially for road bikers.

I observed a particularly interesting anomaly while imaging, considering it didn’t look like

carbon fibers or the polymer. It looked more like sparkles than anything else (Figures 14 and 15).

Out of curiosity again, I did an EDS analysis to see if I could identify what it actually was. Due

to the high content of Potassium and Chlorine in the exact area of the ‘sparkles’, I determine it

must have been some potassium chloride (KCl) salt contamination from my hands or from one of

the people that had handled it before me, but it was very awesome to find some crystals formed

to the surface of the carbon composite material. There was also some sodium in the sample,

which may or may not have contributed in coincidence with the chlorine and formed a salt, but

the shape of the salt crystals was definitely not the orientation of sodium chloride.

After imaging these samples, I couldn’t find much in respect to the cause of warping of this

material on the macro scale. It could have been attributed to the difference in layer widths in

Figure 12, or due to the slight difference in width across the same layer in the same figure.

Carbon fiber reinforced polymers are increasingly being used in new technologies and are an

important step for up and coming engineering and scientific applications. The material is still

quite expensive in comparison to traditional materials (i.e. steel), so hopefully we can find a way

to more easily prepare and create these materials to expand their use in the future. Carbon’s

brittleness in comparison to other materials makes one think they shouldn’t be using it, but along

with a polymer, carbon fiber and carbon nanotube composites could be called the material of the

future.

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Images

Figure 1 Epoxy resin layer, M = 180x, Vacc = Analytical

Figure 2 Carbon fibers going long ways, M = 2000x, Vacc = Analytical

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Figure 3 Carbon fibers, charging, and sand lines going diagonal upward toward the top, M = 600x, Vacc = Analytical

Figure 4 Carbon fibers and charging (top), M = 1200x, V = Analytical

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Figure 5 Image depicting where I used EDS, M = 500x, Vacc = 15 kV

cps/eV

S
3 O
C S

0
2 4 6 8 10 12 14
keV

Figure 6 Graph of EDS analysis of Figure 5 image

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Figure 7 Elemental layout for EDS, Elements as labeled by color

Figure 8 Break down of Carbon, Sulfur, and Oxygen in sample

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El AN Series Net unn. C norm. C Atom. C

[wt.%] [wt.%] [at.%]

-------------------------------------------

C 6 K-series 88723 83.62 83.62 88.23

O 8 K-series 5532 13.34 13.34 10.56

S 16 K-series 13404 3.05 3.05 1.20

-------------------------------------------

Total: 100.00 100.00 100.00

Above – Elemental analysis quantification

Figure 9 Polyphenylene Sulfide, from Wikipedia

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Figure 10 Width Measurement, M = 600x, Vacc = Analytical

Figure 11 Width Measurement, M = 500x, Vacc = Analytical

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Figure 12 Width Measurements, M = 150x, Vacc = Analytical

Figure 13 Fracture of carbon fibers, M = 1800x, Vacc = Analytical

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Figure 14 Salt, M = 1800x, Vacc = Analytical

Figure 15 Salt, M = 5000x, Vacc = Analytical

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Figure 16 Where EDS was performed, M = 5000x, Vacc = 15 kV

cps/eV
1.6

1.4

1.2
S
Cl
1.0 K
O S
C Na Cl K
0.8

0.6

0.4

0.2

0.0
2 4 6 8 10 12 14
keV

Figure 17 Graph of EDS of Figure 16

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Figure 18 Elemental layout for EDS, Elements as labeled by color

Figure 19 Breakdown of Carbon, Oxygen, Potassium, Sodium, Chlorine, and Sulfur in sample

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References

[1] - Composite material. (2017, April 15). Retrieved April 26, 2017, from
https://en.wikipedia.org/wiki/Composite_material

[2] - Carbon fiber reinforced polymer. (2017, April 21). Retrieved April 26, 2017, from
https://en.wikipedia.org/wiki/Carbon_fiber_reinforced_polymer#Carbon_nano-
tube_reinforced_polymer_.28CNRP.29

[3] - Khan, S. M., Gull, N., Munawar, M. A., Zia, S., Anjum, F., Iqbal, M. S., . . . Jamil, T.
(2016, May 24). Polyphenylene sulphide/carbon fiber composites: study on their thermal,
mechanical and microscopic properties. Retrieved April 26, 2017, from
http://link.springer.com/article/10.1007/s13726-016-0439-3

[4] - Polyphenylene sulfide. (2017, March 31). Retrieved April 26, 2017, from
https://en.wikipedia.org/wiki/Polyphenylene_sulfide

[5] - Srinivasa, V., Shivakumar, V., Nayaka, V., Jagadeeshaiaih, S., Seethram, M., Shenoy, R., &
Nafidi, A. (2010). Fracture morphology of carbon fiber reinforced plastic composite laminates.
Retrieved April 26, 2017, from http://www.scielo.br/scielo.php?script=sci_arttext&pid=S1516-
14392010000300022

[6] - http://enve.com/

[7] - Liszewski, A. (2016, March 09). Graphene-Infused Bike Tires Automatically Get Softer
While Cornering For Better Grip. Retrieved April 26, 2017, from http://gizmodo.com/graphene-
infused-bike-tires-automatically-get-softer-wh-1763751098

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