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Fiber reinforced polymer characterization

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**Fiber-Reinforced Polymer
**

Composite

Characterization

Nick

1

Abstract

Composites are of great interest in the automotive and aerospace industries because of

their load bearing capabilities coupled with their lightweight design. Style 4180 Glass Fiber

Reinforced Epoxy (Cycom

®

919) was tested using Dynamic Mechanical Analysis (DMA) to

determine its glass transition temperature (T

g

), which predicts when the composite changes

form and loses its effectiveness. This limit was determined graphically to be T

g

= 125.11°C. T

g

is

crucial when choosing materials for specific applications that include high temperatures. Also,

resin burn-off was utilized to determine the fiber volume fraction (FVF) which roughly

correlates to how much strength is gained in the composite when the load carrying fibers are

present. The mean FVF was found to be 0.34543 with a standard of 0.00374.

2

Contents

Abstract –1

Introduction – 3

Methods – 5

Results – 6

Discussion – 8

Conclusion – 11

References – 11

Appendix A – 12

3

Introduction

Fiber-reinforced polymer composites play a big role in load bearing structural

applications in the automotive and aerospace industries. Their high specific strength, the ability

to shape their structure to produce more aerodynamically efficient configurations, and

lightweight designs makes them far superior to conventional materials. [1] Composites

maintain structural integrity and load-bearing capability at elevated temperatures, which is

particularly important in structures located near heat sources such as engines and electronic

equipment [2]. Also, exterior aircraft and spacecraft structures experience high temperatures

due to aerodynamic heating and other phenomena. The high strength-to-weight ratio and

ability to withstand these temperatures make these composites ideal. [3]

Composites refer to a material composed of two or more distinct phases. In the case of

fiber-reinforced composites, which was the subject of this experiment, the two phases are

represented by a fiber and a polymer matrix. The composite specimen under analysis here was

Style 4180 Glass Fiber Reinforced Epoxy (Cycom

®

919).

The fiber reinforcement is the more crucial component because it provides the strength

and stiffness in the composite. The fibers carry the in-plane loads and also reduce the

coefficient of thermal expansion for the material. On the other hand, the polymer matrix holds

the filaments in place and transfers the load between fibers. The matrix is woven through the

fibers similar to the weaving of clothing. The matrix also protects the fibers from damage,

provides transverse strength (compression), and increases toughness and durability [4]. A few

common types of fibers include glass, carbon (graphite), and aramid (Kevlar).

An important parameter to consider for a fiber-reinforced polymer composite is the

glass transition temperature, T

g.

This temperature can be thought of as the temperature at

which polymer chains can partially move, known as local segmental motion. Below this

temperature, the bulk polymer behaves as a glass which is more or less brittle, and rigid. Above

the glass transition temperature, the material transitions to a more “rubbery” state and

behaves like a viscous fluid. This temperature is crucial because once this temperature is

exceeded, the composite’s load-carrying capability is drastically reduced, basically rendering it

useless. To determine the glass transition temperature, the storage modulus of the material is

analyzed as it is subjected to cyclic deformation as temperature is increased.

Additionally, there are a few important terms to consider. The storage modulus

measures the ability of a material to store energy. On the contrary, the loss modulus measures

the ability of a material to dissipate energy lost to viscous flow. Also, tan delta refers to the

4

(1)

(2)

(3)

dissipation of energy in a material under cyclic loading. Tan delta is shown in this lab as the

phase difference between strain and stress when the material is stressed cyclically.

Another important parameter of a composite is the fiber-volume fraction, which relates

the relative volume of the fibers to the overall volume of the composite material. The volume

fraction is given by:

where

is the volume of the

constituent, and

**is the volume of the composite.
**

In the case of a continuous fiber reinforced polymer, which this lab analyzed, the total

volume fractions should add up to 1, as shown in the following relation:

**Where f, m, and v represent the fibers, matrix and voids respectively.
**

The volume of fibers relative to the matrix is dependent on a number of factors,

including fabrication process, cure cycle, initial volume of fiber and matrix, and fiber packing

arrangement. Generally, the composite failure stress increases linearly with increasing fiber

volume fraction. Also, the impact strength and shear strength of the composite both increase

with increasing fiber volume fraction mainly because the fiber strength is much greater than

that of the matrix. Ideally, the void content should be less than 5% and the fiber volume

fraction should be around 40-70% to ensure the polymer composite maximizes its strength

potential.

Once volume fractions are known, the upper limit of the modulus of elasticity of the

composite can be found. Shown in Equation (3), the rule of mixtures is shown as follows:

**where E represents the elastic modulus, is the volume fraction, f or m represents the fiber
**

or matrix, and “1” refers to the composite material as a whole in the direction of the fiber. The

rule of mixtures is a basic attempt to determine the overall properties of a composite based on

the properties of its constituents. Equation (3) is only valid in the longitudinal direction of

continuous fibers, however the material in this experiment is ‘balanced’ so direction is not

important.

The objective was to find the two important parameters, fiber volume fraction and glass

transition temperature, of the specified fiber-reinforced composite. The fiber volume fraction

was found by a method known as resin-burn off and was expected to be around the 40-70%

5

mark, considering this material is used in aerospace applications. After measuring the weight of

the composite samples, the matrix was burned off and only the fibers were left, which allowed

for the determination of the fiber weight and the subsequent byproducts. The glass transition

temperature was found by the use of dynamic mechanical analysis (DMA). This value was

expected to be reasonably high and was used to determine suitable applications for the

material. Also, a literature value was found and used as a reference to determine the accuracy

of the experiment.

Method

10 samples of Style 4180 Glass Fiber Reinforced Epoxy

(Cycom

®

919) were used in the two parts of this lab. One was

used in the DMA to determine the glass transition temperature

of the material and the nine remaining were used to determine

the fiber volume fraction by the process of resin burn-off

The DMA was done by use of a Q800 DMA made by TA

Instruments shown by Figure 1 to the right. This machine utilized

multi-frequency iso-strain to subject the specimen to a cyclic

load at an increasing temperature. The frequency was 1Hz and

the amplitude of strain was 15 micrometers. Also, the

temperature was started at 25C and increased to 160C at a

ramping step at 5C/min. As the process progressed, the data

was collected through a computer program that allowed for

a plot of the data for analysis.

The resin burn-off method was used to

determine the fiber volume fraction. Initially, the

nine samples were measured by length, width,

and thickness to find the volume and then

weighed. These values can be seen in Table 1 in

Appendix A and the samples and precise

micrometers used to take the measurements are

shown in Figure 2 to the left. As shown, the samples were not too large but nine were used and

averages were taken to ensure the results were accurate as possible and were not skewed by

any random occurrences.

Figure 1: DMA machine used to find T

g

Figure 2: Composite Samples and Tools

6

Figure 4: Determination of Glass Transition Temperature

Next, they were placed in an oven at an initial temperature of

321C and then ramped up to 800C after about 45 minutes to

complete the resin burn-off. This process successfully removed the

polymer matrix because of the differing melting points of the

constituents. The fiber has such a high melting point that it can

withstand the 800C temperature while the matrix cannot. The fibers

were the only things that remained when removed from the oven and

they were subsequently weighed. A Mettler Toledo digital scale was

used for measuring the weights throughout the lab and is shown in

Figure 3 to the right. This scale was extremely precise and was

sensitive to the smallest vibrations so extreme care was exercised.

From the data collected, the fiber volume fraction and

matrix volume fraction were able to be determined using

Equation (1). Additionally, the mean, standard deviation,

variance, and coefficient of variation was found for the fiber

volume fraction.

Results

The DMA produced a large set of data that included variables such as time,

temperature, storage modulus, loss modulus, stress, and tan delta among others. The variables

of interest were plotted below and consist of temperature vs. storage modulus, loss modulus,

and tan delta.

Figure 3: Digital Scale Used in Lab

7

Figure 4 represents the change in storage modulus and loss modulus as temperature

was increased. As shown by the black lines, tangent lines were drawn to the two linear portions

of the storage modulus line. The intersection of these two tangent lines is the glass transition

temperature, which was found to be T

g

= 125.11°C. Also of importance was the change in tan

delta as temperature increased, which is shown in Figure 5 below:

The second part of the lab, done to determine the Fiber Volume Fraction and the Matrix

Volume Fraction, was completed by resin burn-off and a series of weighing the samples with an

extremely precise digital scale. To begin, the 9 samples were weighed and measured in all three

dimensions to determine their volumes. These values are shown in Table 1 in Appendix A. Next,

the samples underwent resin burn-off to remove the matrix polymers, which left only the

fibers. These fibers were weighed and the weights are shown in Table 2 as follows:

Table 2

Sample 1 2 3 4 5 6 7 8 9

Fiber

weights(g) 0.2590 0.2640 0.1871 0.2588 0.2728 0.2572 0.2454 0.2520 0.2671

Figure 5: Increase of Tan Delta as Temperature Increased

8

Using the density of the fiber, 2.48g/cc, the fiber volumes were easily calculated using

Equation (1) and are shown in Table 3 in Appendix A. More importantly, the fiber volume

fractions were found and are listed in Table 4 as follows:

Table 4

Sample 1 2 3 4 5 6 7 8 9

Fiber Volume

Fraction 0.3513 0.3463 0.3380 0.3424 0.3462 0.3440 0.3462 0.3480 0.3467

Along with these values, some statistical information was calculated and is shown in Table 5:

Table5

Fiber Volume Fraction Stats

Mean 0.34543

Standard Deviation 0.00374

Variance 0.00001

Coefficient of Variation 0.01083

Based on the weights of the fibers, the weights and volumes of the matrix could be

determined by subtracting the fiber weights from the overall sample weights and using the

density of matrix polymers at 1.31 g/cc. These values are shown in Table 6 in Appendix A. Also,

the matrix volume fractions were found and are listed in Table 7 below:

Table 7

Sample 1 2 3 4 5 6 7 8 9

Matrix Volume

Fraction 0.4990 0.5133 0.5003 0.4916 0.5069 0.4985 0.5119 0.5074 0.4914

Discussion

The objectives of this lab were carried out in two parts, first with DMA and then by resin

burn-off. T

g

, the glass transition temperature, and the combination of Fiber Volume Fraction

and Matrix Volume Fraction were found in these two sections respectively. These parameters

reveal a lot of information about the material of interest, Style 4180 Glass Fiber Reinforced

Epoxy (Cycom

®

919). Suitable applications and situations of certain failure can be determined by

these critical parameters.

In part one of the lab, T

g

was found graphically to be 125.11C. This was done by

analyzing Figure 4 and using tangent lines drawn from the linear portions of the storage

9

modulus curve. Although a literature value of T

g

for the exact epoxy used in this lab could not

be found, values of around T

g

=127°C were found for glass/epoxy fiber-reinforced composites

[5]. Therefore, the graphically determined value of 125.11°C can be assumed to be fairly

accurate. However, this method does have the potential to include some systematic error. The

error stems from the tangent lines that are drawn from the “linear” portions of the curve,

which leads to imperfect results since these locations are left up to the user to decide. The

intersection of these lines should be reasonably close for most tangent lines, but an error of

less magnitude will most likely be incorporated.

Nevertheless, Figure 4&5 shown in the results depict the data that was gathered during

DMA. By definition, the storage modulus and loss modulus curves are opposites of each other.

Similarly, tan delta is basically the loss modulus divided by the storage modulus, so it follows

the same basic path of the loss modulus itself. All three of these curves changed exponentially

when the glass transition temperature was approached because of the nature of the

experiment. The storage modulus represents the elastic portion which is why it starts out high,

and the loss modulus represents the viscous portion, which is why it starts out low. As the test

progressed, the composite moved closer and closer to the viscous portion which is why the loss

modulus increased and the opposite for the storage modulus. As it reached T

g

, the curves

dramatically change and the composite eventually enter the fully viscous portion and is

rendered useless in load bearing situations.

The second process was done mainly to determine the Fiber Volume Fraction of the

material. The average FVF was found to be 35.453% which is less than what was expected,

considering most composites have a FVF of around 40-70%. Also, the matrix volume fraction

was found based on the burned off weight of the matrix and had an average of 50.23%. Based

on Equation (2), this would lead to the determination of a void volume fraction of about 15%,

which is certainly too high. The void content is important to consider because it refers to the

spacing in between the fibers and matrix. Fatigue test results indicate that voids have a large

detrimental effect on the fatigue life of composite structures if the void content surpasses a critical

value. [6] Although it was not found in this lab, most composites have a void volume fraction of

under 5%

The void volume fraction was initially assumed to be around 2.5% to begin with, so

somewhere in the process the data can assumed to have been skewed. The potential sources of

error that would have altered this value could have come from the weighing of the samples.

One observation that was made during the experiment was the difference in fiber weights that

was found based on the two possible methods. The fiber weights were found after resin burn-

off by simply weighing what was left of the sample after it was heated. However, the fiber

10

weights could have been found by simply subtracting the crucible weight from the

crucible+fiber weight which was also weighed after heating. The two methods would

theoretically produce identical results, however an average difference of 0.0056g was found

between the two methods. This difference is intriguing, but may be explained by the

assumption that the lower magnitude of weight of the fibers was not accurately distinguished

when compared to the weight of the crucible. The direct weighing of the fibers is a better

approach that does not include this error.

The rule of mixtures, shown by Equation (3), can be used to determine the overall

properties of a composite based on the properties of the fibers and the matrix. It can be a good

rule of thumb, but it is not always precisely valid. The composite properties were not explicitly

calculated in this lab because of the many shortcomings of this “rule”, which are explained as

follows. First, the matrix and fiber structures could be altered in the fabrication of the

composite which may lead to initial residual stress in the material [7]. More importantly, the

differential contraction from cooling that occurs after fabrication may cause the matrix to begin

plastic deformation, which would dramatically change the overall properties of the composite

[8]. In short, the rule of mixtures should be used as a guideline but never an exact

measurement because the changes that may occur during fabrication will cause the properties

of the combined constituents to differ from the properties of the isolated fibers and polymers.

As mentioned, there may have been a few sources of error pertaining to the fiber

volume matrix and its byproducts. Averages were taken in most cases to diminish the effect of

human error in weighing and measuring the samples, but it is the nature of the experiment to

experience some error. Nevertheless, the DMA, done by a highly accurate machine, did

produce a glass transition temperature of 125.11°C that was close to the literature value. This

T

g

value is more critical in determining applications for the composite anyway. If one was to

decide whether or not to choose Style 4180 Glass Fiber Reinforced Epoxy (Cycom

®

919), the

glass transition temperature should be the one of the first properties to consider. To be safe, if

the environment did reach around 100°C, it would be unwise to choose this material

considering the consequences that could result if an outlier temperature was experienced near

T

g

. The composite would lose almost all effectiveness if it shifted into a “rubbery” state and

considering the load bearing applications it is used in, this may lead to disaster.

11

Conclusion

The analysis of Style 4180 Glass Fiber Reinforced Epoxy (Cycom

®

919) resulted in a

deeper understanding of composites and how their properties may or may not be suitable for

certain applications. Composites contain specific fibers that greatly increase the overall

strength of the material which makes them perfect for load bearing structures in the

automotive and aerospace industries. The fiber volume fraction is a crucial parameter that

roughly determines the increase in strength that the composite experiences. The FVF of the

material of interest was calculated to have a mean of 0.34543 with a standard of 0.00374. Also,

the glass transition temperature is the key parameter that predicts when the composite will

shift from a rigid, load bearing material to a fluid like state with no real effectiveness. This was

determined graphically by analysis of the temperature vs. storage modulus plot and found to

have a value of T

g

=125.11°C.

References

[1] Progress in Aerospace Sciences. Soutis,C. Feb. 2005.

http://www.sciencedirect.com/science/article/pii/S0376042105000448

[2] http://en.wikipedia.org/wiki/Carbon-fiber-reinforced_polymer

[3] https://www.princeton.edu/~ota/disk2/1988/8801/880106.PDF

[4] Composite Material Characterization Lab Powerpoint

[5] Composites Science and Technology. Moll, Jericho L. April 2013.

http://www.sciencedirect.com/science/article/pii/S0266353813000717

[6] Composite Structures. Muller, Sergio Frascino. 1994

http://www.sciencedirect.com/science/article/pii/0263822394900442

[7] http://www.mech.utah.edu/~rusmeeha/labNotes/composites.html

[8] On the Applicability of the "Rule-of-Mixtures" to the Strength Properties of Metal-

Matrix Composites. Chawla, K. K.

1974http://www.sbfisica.org.br/bjp/download/v04/v04a25.pdf

12

Appendix A

Table 1

Sample 1 2 3 4 5 6 7 8 9

Sample weight (g) 0.4533 0.4707 0.3334 0.4551 0.4838 0.4541 0.4371 0.4461 0.4671

Sample Volume (cc) 0.2973 0.3074 0.2232 0.3048 0.3178 0.3015 0.2858 0.2920 0.3107

Table 3

Sample 1 2 3 4 5 6 7 8 9

Volume of Fibers

(cc) 0.1044 0.1065 0.0754 0.1044 0.1100 0.1037 0.0990 0.1016 0.1077

Table 6

Sample 1 2 3 4 5 6 7 8 9

Matrix

Weight (g) 0.1943 0.2067 0.1463 0.1963 0.2110 0.1969 0.1917 0.1941 0.2000

Matrix

Volume (cc) 0.1483 0.1578 0.1117 0.1498 0.1611 0.1503 0.1463 0.1482 0.1527

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