NEW CARBON MATERIALS

Volume 35, Issue 1, Oct 2020

Online English edition of the Chinese language journal

Cite this article as: New Carbon Materials, 2020, 35(1): 42-49 RESEARCH PAPER

The relationship between the mechanical properties and

microstructures of carbon fibers
Mei-ling Wang 1, Wen-feng Bian 1,2
1
Harbin Institute of Technology, Harbin 150001, China;
2
National Engineering Laboratory for Carbon Fiber Preparation and Engineering, Weihai 264200, China

Abstract: The difference of microstructure of carbon fibers is subtle for the carbon fibers with similar mechanical properties. The mechanical
properties and microstructures of six carbon fibers were investigated by a universal material testing machine, X-ray diffraction, small angle X-ray
scattering and Raman spectroscopy to reveal the microstructure-dependent tensile strength of carbon fibers. Results indicate that the tensile strength
increases with decreasing d002 and ID/IG and with increasing Lc for the five of the six carbon fibers. The dispersion of the tensile strength characterized
by the Weibull modulus increases with increasing micropore radius. The Griffith theory over-estimates the tensile strength of the six carbon fibers.
A more accurate formula was proposed based on the experimental tensile strength and microstructure of carbon fibers
using Mathematics & MATLAB as the simulation tools, which takes into account of the tensile strength loss due to imperfections in the outer-
surface and in the inner-surface, defects and the dispersion of fibers, and is validated by T300 data from other researchers.

Key Words: Carbon fiber; XRD; Weibull; Element; Microstructure

1 Introduction

In the engineering applications of carbon fiber resin matrix that researchers have spent much of their time on different
composites (CFRPs), one or more carbon fibers are likely categoiesy of carbon fibers and ignored the existence of subtle
considered to design composites to satisfy the usage performance differences in the same type of a carbon fiber from
requirements. However, the prediction of the composite different manufacturers. Another is that users often need to
mechanical properties remains a challenging issue because of judge and select carbon fibers with similar properties or similar
the complex microstructures of carbon fibers [1–3]. Conventional products from different manufacturers. The influence of the
theories and methods such as the Griffith’s fracture theory [4], microcosmic structure in the use of the macroscopic properties
Peirce’s weak section theory [5] and Weibull’s distribution of carbon fibers can be the basis of judgment.
theory [6], have been proposed to explain and analyze the
mechanical properties of carbon fibers. These theories are
concentrated on the study of the defects or weak sections of
fibers, assuming that the factors affecting the mechanical
properties of carbon fibers are defects or weak sections that
exist in carbon fibers and the tensile strength depends linearly
on the number of defects. Weibull’s theory also assumes that
defects are the main cause of the discrete fiber strength.
The carbon fiber is generally recognized as a biphasic
system composed of turbostratic graphite crystallites and Fig. 1 The carbon fiber crystal structure model and tensile fracture
micropores. The faulty packing of the crystallite bundle creates mechanism. (a) The turbostratic graphite microstructure of the carbon
spaces between the microfiber bundles in the form of pores or fiber, (b) tensile stress causes a basal rupture along the La┴ direction
holes. Fig. 1 shows a crystal structure model of a carbon fiber and cracks to propagate in the La┴ and Lc directions and (c) as the
and the tensile fracture mechanism, the process of damaging is stress continues to increase, a damaging fracture occurs when the
clearly demonstrated as the stress continues to increase. Based fracture size exceeds the critical value [7].
on the above theory, six PAN-based carbon fibers with similar
properties were studied. We chose six PAN-based carbon fibers
with similar properties as the samples for two reasons. One is

Received date: 31 Dec 2019; Revised date: 23 Jan 2020

*Corresponding author. E-mail: bianwf@163.com
Copyright©2019, Institute of Coal Chemistry, Chinese Academy of Sciences. Published by Elsevier Limited. All rights reserved.
DOI: 1016/ S1872-5805(20)60474-7
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49

2 Experimental when m is large. All data of the Weibull modulus is processed

with EXCEL and the relevance of data is analyzed with the
The following six carbon fibers were used in this study. origin 8 software.
They are (i) high-strength PAN-based SY300 carbon fibers
The section morphology of carbon fibers was obtained
prepared in our laboratory and (ii) high-strength PAN-based
with a JSM-6390 scanning electron microscope. The
commercially available T300, HTS40, A42, TC35-3K and
microcrystalline size and micropore radius parameters were
TC35-24K carbon fibers. Among them, the production process
analyzed using a D/max2500PC X-ray diffractometer (Rigaku
of the precursor fibers for T300 and SY300 was the DMSO–
Co.) using Cu Kα radiation (λ = 0.15418 nm) with a 40 kV tube
H2O method, that for HTS40 and A42 was the ZnCl2–H2O
voltage and a 200 mA tube current. The crystallite interlayer
method, and that for TC35-3K and TC35-24K was the DMF–
spacing, grain size, and porosity were detected using a wide-
H2O method.
angle X-ray detector (XRD). The samples were fixed on a
The diameter of the single carbon fibers, df was measured
fibrous attachment to perform equator scanning and the
using a laser scanning microscope (Aolong, A-5XC) before
micropore radius was detected using a small-angle X-ray
testing.
detector (SAXD). The samples were cut into pieces, pulverized
The density was measured using a density gradient tube.
in a mortar, and placed in a glass tank for scanning. The graphite
Carbon tetrachloride (1.596 g/cm3) was used as the light liquid
crystallite interlayer spacing d002 and crystallite thickness Lc
and dibromoethane (2.179 g/cm3) as the heavy liquid.
were calculated by the following equation (4) and (5) [8–9]:
The mechanical properties of monofilaments were tested
using a universal testing machine (Instron, 1122) with a gauge
of 25 mm, in accordance with the ASTM-D3379 standard.
There are no less than 30 valid samples and the invalid samples
are determined based on （1）abnormal curve, （2）breaks at where θ is the scattering angle, λ is the wavelength of the
the end not in the middle of the sample and（3）abnormal data. X-ray and K is the shape factor [10].
For example, two fibers are superimposed to make the data of
The micropore radius (r) was obtained by the Guinier
the sample too huge.
principle. The InI(h)–h2 curve is a straight line when h is small
According to the Weibull weakest connection theory and [11–12]
. The slope −Rg2/3 is obtained by fitting the linear portion
datum statistical methods, a carbon fiber is assumed to be ideal
with the Guinier formula [Fo. (6)], assuming that the micropores
single fracture morphology that has only one type of defect. The
in the carbon fiber were considered spherical. r was calculated
carbon fiber diameter is uniform and has a circular cross-
using the Equation (7). All data of XRD and SAXD were
section. When the stress field of carbon fiber is uniform, the
processed with the jade 5 software.
one-dimensional double parameter Weibull calculation
equations (1) and (2) are as follows [14–16]:

The degree of graphitization was estimated with a HR800

where P is the survival probability of fibers, F is the
fracture probability of fibers, L is the effective length of the
standard test paper frame, σ is the fiber strength, σ0 is the
normalization factor, m is the form factor (also known as the
Weibull modulus), N is the total number of measured carbon
fiber monofilaments, and R is the number of fragmented
monofilaments at or below a stress level σR.
The logarithm of both sides of Eq. (1) leads to the
following linear equation (3) :
Thus, m, the discrete strength of carbon fibers, can be
obtained through linear regression from the Weibull plot of
Equation (3). The strength dispersion of carbon fibers is small
spectrometer (HORIBA Co., France) at room temperature in a
nitrogen atmosphere using a 457 nm Ar laser as a laser source.
R (=ID/IG) was used to evaluate the graphitization of materials.
ID is the D band peak intensity of the Raman spectrum at
1 360 cm−1 and IG is the G band peak intensity of the Raman
spectrum at 1 580 cm−1 [13]. All Raman data were processed with
the Labspec5 software.
3 Results and discussion
3.1 Mechanical properties
Table 1 lists the tensile strength at a gauge length 25 mm
of six carbon fibers. A42 has the highest tensile strength and
T300 has the lowest tensile strength. In the datum sheet
provided by the producer, the six carbon fibers have the same
average diameter of 7.0 μm. However, the actual diameter
deviation is very large and the maximum diameter of TC35-3K
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49

is 7.69 μm, and the minimum diameter of TC35-24K is 7.13 μm.
Meanwhile, the density is dissimilar. TC35-3K and TC35-24K
difference only in terms of the bundles of filaments, but the
density has a difference of 0.019 g/cm3. The results shown in
Table 1 also clearly indicate that the tensile strength of the
carbon fiber exhibits appreciable scattering. The statistical
distribution of the fiber strengths can be described by the
Weibull modulus. Fig. 2 shows the Weibull plots of the six
carbon fibers. The Weibull modulus m for SY300, T300,
HTS40, A42, TC35-3K, and TC35-24K fibers are 6.394 7,
4.559 7, 6.296, 7.566 5, 5.865 7, and 4.4675, respectively.
A42 has the highest Weibull modulus and TC35-24K has the
lowest.
The volume effect suggests that the smaller the diameter
of the fiber, the less defects in the fiber. That is to say, the
smaller the diameter of a carbon fiber, the greater its tensile
strength, the smaller the dispersion. As seen from Table 1 and
Fig. 2, TC35-24K has the smallest diameter, but the dispersion
coefficient of tensile strength is the largest, the Weibull
modulus is the smallest，and the tensile strength ranks the fourth.
It is completely inconsistent with the theory. To get full
appreciation of data in Table 1, there is no correlation between
the Weibull modulus, diameter and the tensile strength for
carbon fibers with similar properties. In fact, the diameter of the
carbon fiber cannot be constant when the Equation (1) is used
for calculating Weibull modulus. From this view, the diameter
should be related to the dispersion of carbon fibers. But for
carbon fibers with

Table 1 Physical and mechanical properties of carbon fibers.

a
: Producer’s data sheet, the number in () indicates the standard deviations

Fig. 2 Weibull plots of PAN-based carbon fibers at a 25-gauge length: (a) SY300, (b) T300, (c) HTS40, (d) A42,
(e) TC35-3k, and (f) TC35-24K.
reflected in the nanometric, the volume effect is not obvious
similar properties, the difference in diameter is only
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49
and there is no dominant rule. The production process of
carbon fibers is long, each step can lead to defects, in
addition to the difference in macroscopic physical properties
and microstructure. We believe that the tensile strength and
dispersion of carbon fibers with similar properties are
caused by crack propagation and the differences in defects
are related to the differences in microstructures and
morphologies.
Fig. 3 The section morphology of carbon fibers.
3.3 X-ray diffraction analysis
Fig. 4 shows the XRD patterns of six carbon fibers that are
observed via the equatorial scan, from which the crystallite
thickness Lc and the crystallite interlayer spacing d002 are
calculated according to Equations (4) and (5), respectively. The
literature [8] revealed that Lc increased and d002 decreased with
the increment of the tensile strength, this graphitization
behavior is due to the increasing degree of graphitization of the
carbon fibers caused by the molecular mobility and structural
rearrangement. The main factors that influence the Lc and d002
are the heat treatment temperature. The relationship of the
tensile strength with Lc and d002 are plotted in Fig. 5 and the
results show a slow increase in Lc and decrease in d002 as the
tensile strength increases except for SY300. The order of this is
T 300, TC35-24K, TC35-3K, HTS40, A42. The most obvious
difference between SY300 and T300 is the difference in density.
Compared with the four other carbon fibers, the carbon fiber
3.2 Cross-section morphology
As can be seen in Fig. 3, the cross-sections of (a)SY300
are mainly ellipses, (b) that of T300 include nearly round,
elliptic and kidney shapes, (f) that of HTS40 are nearly round,
and that of (c)TC35-3k, (d)TC35-24k and (e)A42 are mainly
kidney-shaped. The irregular cross-section makes the diameter
of carbon fiber discrete. But as shown in Table 1, the standard
deviation of the diameter of carbon fibers with a non-circular
cross-section morphology is not necessarily large. The standard
deviation of diameter of A42 is smallest and its cross-section
morphology is uniform.
with the same precursor fiber production process that has a
higher density and tensile strength has a more perfect
microcrystalline structure, e.g. HTS40 and A42, TC35-3K, and
TC35-24K. Although the microcrystalline structure of T300 is
more perfect, it is less dense than SY300, which means that the
compactness of SY300 is slightly worse, and there are more
micropores in the microstructure, which reduces its strength.
3.4 Raman spectroscopy analysis
Fig. 6 shows the Raman spectra from the surface of the
carbon fibers. The degree of structural disorder (also called the
degree of graphitization) of fibers can be characterized by the
ratio of the integrated intensity of the disorder-induced band
(ID(1360 cm-1)) to the Raman-allowed band (IG(1 580 cm-1)),
which describes the degree of disorganized material in the
carbon fibers, and the formula is as follows:
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49
Fig. 4 X-ray diffraction patterns of carbon
fibers in the equatorial scan.
Fig. 5 Relationship of tensile strength with d002 and the
Lc of carbon fibers.
Fig. 6 Raman spectra taken from the surface of carbon fibers.
As shown in Fig. 7, there is a decrease in R with increasing
the tensile strength except for SY300, the order is T300, TC35-
24K, TC35-3K, HTS40, and A42, which has the same variation
trend as d002. The R values of T300 and SY300 are obviously
much larger than the other four carbon fibers and the tensile
strengths of T300 and SY300 are lower than the other four
fibers. As shown in Fig. 8, the measurement of the X-ray
diffraction is the inner-surface and core part of the carbon fibers
and the Raman spectra is quite limited in the outer-surface part.
For the six specimens with similar properties, the degree of
graphitization in the outer-surface of carbon fibers is the same
as that in the inner-surface and core.
Fig. 7 Relationship between the tensile strength and the R values of
carbon fibers.
Fig. 8 Schematic illustration of the three-layer structure of a carbon
fiber consisting of a core, inner-surface, and outer-surface [18].
3.5 Small-angle X-ray diffraction analysis
According to the Equation (6), the InI(h)–h2 curve is
shown in Fig. 9 and the micropore radius of carbon fibers can
be calculated by the Equation (7). As shown in Fig. 10, for
carbon fibers with the same production process for
precursor fibers, the micropore radius decreases as the tensile
strength increases in a manner that is consistent with the
density changing trend. This can also be used to explain why
the graphitization structure of SY300 is worse than that of T300
yet the tensile strength of SY300 is higher than T300 .
The carbon fibers with a larger micropore size is more
likely to form stress concentrations under the action of tensile
stress,which results in the reduction of the tensile strength. As
shown in Fig. 11, the micropore radius decreases as the Weibull
modulus increases and the order is TC35-24K, T300,
TC35-3K, HTS40, SY300, and A42. Thus, it can be concluded
that the micropore radius is one of the main reasons for the
difference in the Weibull modulus of carbon fibers with similar
properties. At the same time, comparing the fiber diameter with
the micropore diameter, the difference in fiber diameter do not
directly affect the size of micropores, which is consistent with
the result of 3.1.
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49
Fig. 9 The relationship between lnI(h) and h2.
Fig. 10 The relationship between the tensile strength and the
micropore radius of carbon fibers.
Fig.11 The relationship between the Weibull modulus and the
micropore radius of carbon fibers.
3.6 Presentation of estimation formula of the tensile
strength of carbon fibers
It is well known that the tensile strength of carbon fibers
is greatly influenced by the presence of flaws and defects [18-21].
In the process of studying the mechanical properties of carbon
fibers, scientists have been trying to find a way to estimate the
tensile strength. However, it has not been found the most
suitable method and theory. At present, the most common
theory is the Griffith (Irwin) formula, which gives the
relationship between the tensile strength and crack tip radius:
Where σu is the estimated tensile strength, KIC is the
fracture toughness and taken as the same value 1.25
MPa·m1/2[22], Y is geometric constant for a crack and taken as
0.75 [23] and C is the radius of a sharp-edged crack.
The Griffith,s theory is used to calculate the strength based
on the following two assumptions. (1) Carbon fibers can be
modeled as a composite structure composed of microfibers,
microcrystals and micropores [24], so carbon fiber can be
considered to be isotropic. (2) Hemispherical defects are used
in sample making with the assumption that the crack of carbon
fiber is ellipsoidal.
It’s worth noting that carbon fiber is distinctly anisotropic.
Moreover, the diameter of micropores is not the direction of
fracture. As seen from Table 2, the difference between the
tensile strength calculated by the Griffith theory and the actual
tested is huge, the σu-σ of T300 is 2 345 MPa. But, the tensile
strength calculated by the Griffith theory of six carbon fibers
are similar and the difference between the highest A 42 and the
smallest TC35-24K is only 276 MPa. It is considered that the
defect is the most important factor that affects the mechanical
properties of carbon fibers. However, defects are not the only
factor, they are also related to the degree of the graphitization
of carbon fibers, its imperfect structure, and its own coefficient
of variation. This is the main reason why the measured data are
much smaller than the theoretical calculated ones.
In summary, the over estimation of the tensile strength of
carbon fibers by the Griffith and Weibull theory can be caused
by the loss of tensile strength by microstructural factors.
According to the experimental results in this paper, we propose
an expression to describe the tensile strength of the carbon
fibers by the equation (9):
σ = 5679 - σ R - σ d - σ r - σ m - χ （9）
Where σ is the actual strength of carbon fibers, 5,679 is
the average tensile strength calculated by Griffith theory of the
six specimens, σR is the strength loss due to imperfections in the
outer-surface, σd is the strength loss due to imperfections in the
inner-surface, σr is the strength loss due to defects, σm is the
strength loss due to the dispersion of fibers and x is other factors
that affect the tensile strength.
Based on the Griffith and Weibull theory and with the
n u m e r i c a l s i m u l a t i o n a n d a n a l y s i s u s i n g Mathemat
ics & MATLAB, the equation (9) can be re-expressed as the
equation (10):
12.76
78716
σ = 5679 - 14107 R + 222072d 002 - - 11.48 m - 45579 (10)
r
 Mei-ling Wang et al. / New Carbon Materials, 2020, 35(1): 42-49
It can be seen that the equation (10) is a systematic
estimation model and is not composed of the proportional
distribution of each microstructure factor. According to the data
of T 300 carbon fibers given by other researchers, R is 1.08 [25],
d002 is 0.354 5 nm [26], r is 15.4nm [27] and m is 6.13 [14], the
estimated tensile strength is 3 369 MPa, which is close to 3 530
MPa given by Toray and also consistent with the T300 tensile
strength tested in this paper. It is worth mentioning that 3 530
MPa is usually the tensile strength of multifilaments in carbon
fibers, while the tensile strength of carbon fiber monofilament
is generally small, which is also consistent with the estimated
results. The equation (10) can be used to determine the
correlation between mechanical properties and
microstructure of T300 level carbon fibers.Table 2 Tensile
strength estimation for carbon fibers.
4 Conclusions
For carbon fibers with similar properties, the degree
ofFig. graphitization on their outer-surface is different from that
in the inner-surface and the central part, but the graphitization
degree on the outer-surface and central part present the same
change trend with the tensile strength. The higher the degree of
graphitization (the higher the Lc, the smaller the d002 and R), the
higher the tensile strength of carbon fibers.
The correlation law between the density and tensile
strength is the same as the micropores and tensile strength in
that that the density and micropore radius decrease as the tensile
strength increases when carbon fibers are prepared from the
same precursor with the same method, such as T300 and SY300,
TC35-24K and TC35-3K, and HTS40 and A42.
There is a significant linear correlation between the
micropore radius and the Weibull modulus of carbon fibers. The
micropore radius decreases as the Weibull modulus increases.
Based on the experimental data of the mechanical
properties and microcosmic structure, the tensile strength of
carbon fibers can be simulated and analyzed numerically
using Mathematics & MATLAB to obtain a formula that
matches the real condition through the comparison of T300
data from other researchers.
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