Original article

Textile Research Journal

2018, Vol. 88(17) 1943–1953

Investigation of the mechanical properties ! The Author(s) 2017

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of lignin nanofibrous structures using DOI: 10.1177/0040517517715080
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statistical modeling

Seyed Abdolkarim Hosseini1,2, Li-Ting Lin2 and Frank Ko2

Abstract
The growing use of nanomaterials, environmental concerns and related industrial applications have provided unique
opportunities for the development of nanofibers from natural biopolymers such as lignin. The main purpose of this study
was to develop a direct relationship between lignin single nanofiber, the aligned nanofiber mat and the twisted nanofiber
yarn’s strength using the weakest link theory of strength and the statistical model proposed for parallel fiber bundles.
Twisted yarn strength was obtained via in situ mechanical properties of yarn constituent nanofibers affected by the
Weibull distribution parameters, fiber fragmentation phenomenon, and obliquity. The results showed that the estimated
strength of the single nanofiber and the aligned nanofiber mat was in a good agreement with the experimental data. As it
might be expected, the yarn’s estimated strength was found to be highly influenced by the fiber fragmentation
phenomenon.

Keywords
weibull distribution, fragmentation phenomenon, lignin, strength, structure-properties, distribution

In the last two decades, research groups have been engineering design of nanofiber-based products, being,
focusing their attention on designing and modifying in fact, an integral part of this field. Although many
nanofibers, with a particular emphasis on the tailored studies have been carried out on conventional textile
physical, chemical, and mechanical properties for a fibers and their fibrous structures, as well as their mech-
variety of applications such as tissue engineering scaf- anical relationship,9 single nanofibers are different,
folds, fuel cells, sensors, filtration and actuators.1–5 In a compared with conventional fibers, as they have a
classical electrospinning system, products are usually in very high specific surface area, high fiber aspect ratio
the form of some mat; however, some researchers have and nanoscale diameters. Therefore, traditional devices
attempted to modify the setup to explore nanofiber- and methodologies employed for characterization and
based structures including the aligned nanofiber mat analysis of nanofiber structural and mechanical proper-
and complex three-dimensional (3D) fiber architecture.5 ties could not be applied readily. Building on well-
In recent years, published studies have shown the bene- established classical textile structural mechanics and
fit of continuous carbon nanotubes yarns such as
reinforcement, and mechanical, electrical and thermal
properties.6,7 Also, fabrication of nanofiber-based 1
Nanotechnology & Advanced Material Institute (NAMI), Department of
yarns, including hollow and core-shell structures, Textile Engineering, Isfahan University of Technology, Isfahan, Iran
from a wide range of polymers in twisted forms can 2
Department of Materials Engineering, University of British Columbia,
have potential applications such as precursors for Vancouver, BC, Canada
carbon nanofibers, suture in biomedical engineering
and conformal finishing on textile yarns with Corresponding author:
Seyed Abdolkarim Hosseini, Nanotechnology & Advanced Material
electrospun nanofibers.8 Evaluation of nanofibrous Institute (NAMI), Department of Textile Engineering, Isfahan University
mechanical properties and the relationship between of Technology, Isfahan 8415683111, Islamic Republic of Iran.
the hierarchical structures can be essential for the Email: hoseinir@[Link]
1944 Textile Research Journal 88(17)

modified analytical methods, we can develop nanofi- that the fiber strength distribution is the Weibull-type.
brous structures. Recently, a fiber-web theory was pre- The main purpose of this study was to investigate the
sented to verify/complement the physical testing results mechanical relationships between the lignin parallel
of the single nanofiber and the randomly oriented nanofiber bundle, the twisted yarn and its constituent
nanofibrous mat through geometrical analysis.10 single nanofiber properties based on the weakest link
There are, in fact, several methods to predict yarn theory and statistical strength. This is likely to lead to a
mechanical properties based on fiber properties. The better understanding of how microscopic mechanical
two approaches often used are mathematical and stat- properties of constituent fibers, strength dispersion,
istical models. The mathematical model is based on fragmentation phenomena, fiber critical length, and
applied physics, adopting certain assumptions, i.e., obliquity can affect the macroscopic responses of bun-
idealized structure, packing and migration, to simplify dles and yarn failure.
the calculation.11 Using this mathematical model has
shown the influence of yarn geometric features such
as yarn helix surface angles and lateral yarn contraction Statistical method
on the translation of fiber strength into yarn
strength.12,13 In practical studies, due to the random
Statistical modeling
nature of textile materials’ geometry and properties, Classical and early studies on the fiber mechanical
the statistical model has been widely used to provide properties were focused on investigating the statistical
the relationship between fiber and yarn mechanical strength of individual fibers based on the weakest link
properties.14 For example, by using two parameters of model, using the Weibull distribution.25–27 Daniels27
Weibull distributions, the relationship between the stat- developed the work and investigated the relationship
istical strength of an aligned fiber mat with its constitu- between the statistical strength of a parallel fiber
ent fibers, strength of ring and air jet cotton/polyester bundle with its constituent fibers, showing that the
yarns was determined as a function of gauge length;15,16 distribution tended to be the normal form. Also, the
there are also some other works regarding continuous results of several important mathematical researches
and spun twisted yarns.17,18 were reported for breaking kinetics based on a statis-
Lignin, which is the second most abundant biopoly- tical theory of mechanical breakdown in a time-depen-
mer on earth after cellulose, is one of the three major dent system and for classical fibers whose strength was
components of vascular plants. It has a 3D amorphous, independent of the rate of loading.28–30 For a parallel
and heterogeneous structure consisting of phenylpro- fiber twisted yarn, Daniels’ mean strength and its stand-
pane units with a brittle nature.19 Lignin is also a ard deviation were modified by directly applying the
byproduct of the pulp and paper industry; different twisting effects.27
pulping processes can generate different types of tech-
nical lignin such as kraft lignin.20 Now most lignin is
burned as fuel, and less than 2% of it is utilized for
Single nanofiber
commercial products such as resins and dispersants.21 A single nanofiber is considered as a chain consisting
Development of high value products from lignin can of several links. According to the weakest link theory or
enhance the value of this underutilized material; one size effect on failure, if a fiber is gradually stretched, it
of the targets is to make some kind of lignin-based breaks at its weakest cross-section.31 For Weibull-type
nanofiber for carbon nanofiber (CNF) precursors. fibers, the cumulative distribution function of ten-
Since lignin is an inexpensive and bio-renewable mater- sile strengths provides the probability that fibers can
ial with high carbon content, it has the potential for break before the strength reaches the value of s. A
making low-cost CNF. In recent years, lignin-based two-parameter Weibull distribution is as follows:25
electrospun nanofibers have been developed.20,22,23
Studies have been carried out on the mechanical prop- "   #
erties of lignin fibers, but most of the research has been l  b
Fl ð Þ ¼ 1  exp  ð1Þ
centered on the fiber mat level, and the translation of l0 Z
the mechanical properties from the single nanofiber to
nanofiber assemblies is still not fully analyzed.6 In order
to develop the application and performance enhance- where s is the fiber tensile strength, Z is the scale par-
ment for the lignin-based nanofiber, the potential rela- ameter, and b is the shape factor for a fiber gauge
tionship between the mechanical properties of the lignin length (l0). The shape factor shows the fiber strength
single nanofiber and nanofibrous assemblies needs to be dispersion, with the higher value of b indicating the
established and compared to that of different nanofiber more fiber strength uniformity. This probability is a
structures. Lignin is a brittle fiber,24 so we can assume continuous function of l and s.
Hosseini et al. 1945

The expected mean value of the fiber strength with factor, which is related to the fiber aspect ratio, Vf is
length, l, can be derived from the expected value of the the fiber-volume fraction , Z is the scale parameter, b is
cumulative distribution function of nanofiber tensile the shape factor, and lc is the fiber critical length. The
strength (Equation 1)32 as follows: orientation efficiency factor depends on the twist angle
at the yarn surface  and the yarn Poisson’s ratio VLT is
 1=   defined as follows:17
l b 1
bf ¼ Z  1þ ð2Þ
l0 b 2ð1  VLT Þ þ ð1 þ VLT Þ sin 2
K ¼ ð6Þ
4
where bf is the expected mean value of the fiber
strength, Z is the scale parameter, and b is the shape Cox has shown that the value of the length efficiency
factor for a fiber gauge length (l0). The coefficient of factor Kl approaches unity if fiber length or fiber aspect
variance (CV) of bf is as follows:32 ratio is large.33
The fragmentation phenomenon in the yarn is a
0   12 process in which the constituent fibers continuously
 1 þ b2
CV ¼ @    1A ð3Þ break during the increase of yarn elongation before
2 1 þ b1 the rupture of yarn; then they are again involved in
building up the yarn strength. For the composite, lc
could be obtained according to the following
equation:34
Tensile strength of an aligned nanofiber mat rf  f
lc ¼ ð7Þ
The tensile strength of an aligned nanofiber mat ( b ) g
with a sufficient amount of fiber has a normal distribu-
tion27 and is related to the fiber scale parameter and where rf is the fiber diameter, sf is the fiber tensile
shape factor. strength, g is the shear strength (the local lateral pres-
The expected mean value of the mat strength is ^b as sure), and  is the friction coefficient between fibers.
follows: Mean lateral pressure on the fibers (g) in the yarn
can be calculated by the following equation:18
 1=  
lb b 1 n
^
b ¼ Z b exp  ð4Þ g¼ Ef y K ð8Þ
l0 b 2

where ^b is the expected mean value of the mat where Ef is the fiber Young’s modulus, y is the yarn
strength, Z is the scale parameter, and b is the shape strain, n is the yarn cohesion factor, which indicates
factor for a fiber gauge length (l0). how the yarn grips fibers, and is calculated according
to the twist angle at the yarn surface,  is the friction
coefficient between fibers, and Ka is the fiber orienta-
Tensile strength of the twisted nanofiber yarn tion efficiency factor due to fiber obliquity.18
The strength of the twisted nanofiber yarn has a normal For the twisted yarn, lc is calculated by the following
distribution, as in an aligned parallel mat. Previous equation:17
research shows that several parameters can influence
the tensile properties of yarn. The scale parameter 2rf  f
lc ¼ ð9Þ
and the shape factor are two important factors nEf y K
influencing the single nanofiber and the mat strength.
Another factor which could be considered is fiber crit- To calculate the surface angle of the twisted yarn,
ical length. the well-known classical equation could be used, as
The expected mean value of the yarn strength (^ y ) is follows:11
as follows:18 2 3
 1=
  40 2
1=b 1  ¼ arctan410  3 5 ð10Þ
^y ¼ K Kl Vf Zðlc bÞ exp  ð5Þ rf V f
b

where Ka is the orientation efficiency factor due to the where a is the twist angle at the yarn surface,  is the
fiber obliquity, Kl is the fiber length efficiency twist factor (tex1/2 twist per cm), rf is the fiber specific
1946 Textile Research Journal 88(17)

density, and Vf is the fiber-volume fraction (rbundle/

rpolymer).
Morphological characterizations
Also, yarn strain was obtained according to the fol- F4SKL electrospun nanofiber morphology was
lowing equation:11 examined by using a scanning electron microscope
(SEM, Hitachi S3000N) under high vacuum, with 5 kV
 
f ¼ y cos2   VLT sin2  ð11Þ accelerating voltage, and at 15 mm working distance.

where f is fiber strain, y is yarn strain, a is the

twist angle at the yarn surface, and VLT is the Yarn
Mechanical properties characterization
Poisson’s ratio. Single nanofiber. Single as-spun nanofiber mechanical
testing was conducted using the T150 UTM tensile
tester system (Agilent Technologies, USA). A similar
Materials and methods device was used by Jian.37 Nanofiber samples were
first collected on a Y-shaped metal frame during the
Materials electrospinning process and then transferred to a 5-
Softwood kraft lignin (Indulin-AT; SKL) was mm gauge length plastic template glued with epoxy
obtained from MeadWestvaco (Glen Allen, VA, resin. The Kleindiek nanomanipulator and the
USA). SKL was washed with diluted HCl (pH 2) Olympus LEXT OLS 4000 confocal microscope were
for 30 min  5 to remove water-soluble impurities used for single nanofiber selection to remove fibers until
and ash. The purpose of the acid wash was to get one single nanofiber remained on the template. A total
rid of the impurities in the kraft lignin. There were of 26 samples were tested and the nanofiber diameter
small parts of lignin that could be dissolved in acid was measured for 10 different parts of each sample and
treatment, but most of them were insoluble. The averaged. Figure 1 shows the schematic diagram of
lignin structure had some slight modifications since single nanofiber preparation for the tensile test.
the aliphatic hydroxyl group content and the con-
densed structures of lignin were reduced. After the Aligned nanofiber mat. A tensile test of aligned nanofiber
acid wash, the SKL was dried at 105 C in an oven mats was conducted by using the KES-G1 Kawabata
overnight. Polyethylene oxide (PEO) at 1  106 g/mol micro-tensile testing system at the elongation rate of
was obtained from Sigma-Aldrich, USA. N,N- 0.02 cm/s. Sample strips (5 cm x 0.5 cm) were glued on
dimethylformamide (DMF), methanol and methylene a hollow paper frame with a 4-cm gauge length. The
chloride were all of American Chemical Society paper frame was cut before the test and 12 samples were
(ACS) reagent grade and obtained from Fisher tested (Figure 2). The measured load was recorded by
Scientific (Ottawa, ON, Canada). SKL was first frac- loading voltage and then converted into gram-force.
tionated using different organic solvents and the frac- Engineering stress (MPa) was also calculated.
tionation 4 (F4SKL) part was used as the precursor
material. The fractionation process had been modified Fiber alignment characterization using Angular Power
by the previous research and the molecular weight Spectrum. In this section, the directionality of the nano-
(MW) of F4SKL was 35,000.35,36 fiber mat was explored using image processing tech-
niques in Fourier Transform Analysis (FTA). Any
periodical function with different degrees of complexity
Solutions preparation and the electrospinning setup was transformed into a series of sine and cosine func-
After being isolated and dried, F4SKL was blended tions; further, Spectral Density Function, Fourier
with PEO with a 99:1 weight ratio and dissolved in Power Spectrum (FPS) and Angular Power Spectrum
DMF as the electrospinning solutions. The needle were calculated using FTA. The alignment degree of a
gauge number G25 (corresponding to the needle inner nanofiber mat could be objectively determined by using
diameter of 0.51 mm) in combination with the solution Angular Power Spectrum (APS), based on the SEM
concentration of 25 wt% was applied for electrospin- images of constituent nanofibers. APS was obtained
ning. A positive voltage of 15 kV at the 0.03 ml/min according to the following equation:38
pump speed with the spinning distance of 18 cm was
X
R
used for the electrospinning setup at room tempera- AðÞ ¼ pr ðÞ ð12Þ
ture.23,24 Single nanofibers were collected on a Kato r¼1
tech nanofiber electrospinning unit (NEU), while
aligned nanofiber mats were collected on a NANON- where is a two-dimensional FPS of SEM image
01 A electrospinning unit with the rotating drum speed (N  N pixels), and r and y are the elements of the
of 2000 revolutions per minute (RPM). polar coordinate. The variables of r and y vary from
Hosseini et al. 1947

Figure 1. (a) Schematic diagram of single nanofiber preparation and tensile test, (b) Nanofiber collection, (c) Nanofiber selection,
(d), (e), and (f) Tensile testing.

1 to N/2 and 0 to 2p, respectively. The intensity of the (Figure 3(b)) formed a broad peak around 90  30
APS was normalized by the corresponding mean inten- degrees and the one was around 18 degrees. These fig-
sity of the FPS. Normalized APS versus y showed the ures show the SEM images of random and aligned
degree of the alignment of the nanofiber mat. nanofibers with their corresponding APS, respectively.
In the aligned nanofiber mat, the majority of fibers were
aligned in the fiber length direction.
Results and discussion
Directionality of the nanofiber mat Tensile strength of the single and aligned
nanofiber mat
The use of APS showed that the aligned nanofiber mat
had a prominent peak around 90  6 degrees Figure 4 shows the representative stress strain curve of
(Figure 3(a)), while the random nanofibers mat the lignin single nanofiber and the aligned nanofiber
1948 Textile Research Journal 88(17)

Figure 2. Sample preparation of aligned nanofiber mats for the tensile test.

Figure 3. (a) The aligned nanofiber mat and its corresponding APS; (b) The random nanofiber mat and its corresponding APS.
APS: Angular Power Spectrum
Hosseini et al. 1949

Figure 4. Typical stress strain curve of the lignin single and aligned nanofiber mat.

freedom ¼ 3, resulted in
2 ¼ 1.835, with a p-value of
0.607, showing that the model was significant at the
level of  ¼ 0.05.
By considering l/l0 ¼ 1 and using the maximum like-
lihood technique, the scale parameter (the value of
strength with a failure probability of 63%) and the
shape factor were obtained from the slope of the best-
fit Weibull distribution line, which were  ¼ 41.478 MPa
and  ¼ 3.646, respectively. The shape factor for wood
and tunicate nanofibrils was 0.9 and 1, respectively.39
These indicated that the lignin nanofiber with the shape
factor 3.646 had a more uniform stress distribution
than wood and tunicate nanofibrils.
By using Equations 2 and 3, the mean expected
nanofiber strength (b  f ) and its CV% were estimated
to be 37.403 MPa and 30.47%, respectively. These
values had a good agreement with the mean experimen-
Figure 5. Probability of failure of single nanofiber. tal strength of 27 samples, with 37.468  10.760 MPa
and CV% ¼ 28.724 (Table 1).
mat. The gauge length of the single nanofiber and the The average fiber diameter of the single nanofiber was
aligned nanofiber mat was 5 mm and 4 cm, respectively. 932  139 nm. Also, the single nanofiber Young’s modu-
This figure shows that the rupture of the single lignin lus and the breaking strain were 2428.133 
nanofiber was of brittle type; and it occurred simultan- 889.236 MPa and 0.021  0.006, respectively.
eously at the ultimate tensile strength. Although it was The length-dependent Weibull function showed that
expected that the rupture strength of the aligned nano- with the decrease of the fiber length, the fiber strength
fiber mat would be equal to the breaking strength of the was increased. Figure 6 shows that with decreasing fiber
individual nanofiber, the strength and extension disper- length, the fiber strength was increased and the effect
sion of the single nanofiber caused the aligned nanofi- was more prominent for a length lower than about
ber mat strength to obey the normal distribution.27 300 nm. The strength of a single lignin nanofiber with
Figure 5 shows the lignin single nanofiber strength the diameter of 900 nm and the length 50 nm could be
probability of failure using the Weibull distribution. increased to 900 MPa, showing to be comparable with
Using Pearson’s Chi-square test with degrees of the tensile strength of the stainless steel.40
1950 Textile Research Journal 88(17)

Table 1. Experimental and theoretical results of strength for the nanofibrous lignin  ¼ 41.5 (MPa),  ¼ 3.7

Experimental
Gauge Strength (MPa) Theoretical Strength (MPa)
Length (mm) (CV%) (CV%)

Single nanofiber 5 37.5 (28.7) 37.4 (30.5)

Aligned nanofiber mat 40 14.2 (4.6) 12.5
Nanofiber yarn None Changed from 19.1 to 189.5 MPa
according to the critical length
: shape factor; : scale parameter; CV%: coefficient of variance.

Figure 6. The relationship between the expected strength of the single nanofiber and the fiber length.

The estimated mean strength of the aligned nanofi-

ber mat was 12.503 MPa, by using Equation 4, and the
value showed a reasonable agreement with the experi-
mental mean value of 12 samples ¼ 14.21  0.655 MPa
(Table 1). The ratio of ^b =b
 f (0.334) was low due to the
low value of . If we chose  ¼ 10 (brittle ceramic) and
100 (steel), the value of ^b =b
 f would be equal to 0.613
and 0.972, respectively. These results indicated that
how the fiber strength uniformity affected the mat
strength.

Estimation of the tensile strength of the nanofiber yarn. The

twisted nanofiber yarn strength depends on several par-
ameters such as lignin fiber specific density (1.31 g/
cm3)41 and fiber-volume fraction (Vf ¼ 0.9), according Figure 7. ^ y =b
 f versus lc/l0 for  ¼ 30.
to the previous research).42 The other parameters
including Ka, lc, and n, which were depended on the
yarn surface helix angle (a), could be obtained via yarn volume VLT ¼ 0.5 when the twist factor was chan-
Equations 6 and 9, and the work of Pan.18 Among ged from 30 to 125. When the lateral pressure was low,
them, the key parameter that mainly affected the yarn the fragmentation phenomena could not occur com-
strength was the lc. The estimated yarn strength was pletely, i.e., for  ¼ 30, with decreasing lc from l0 ¼ 5
calculated using Equation 5, by assuming the constant to 0.25 mm, ^y was increased from 19.043 to
Hosseini et al. 1951

Figure 8. Fiber critical length in the fragmentation process versus the yarn strain.

Figure 9. Yarn strength as a function of the fiber critical length.

29.555 MPa (Figure 7), respectively. This indicated that 50 to 350 MPa.43,44 The high ratio of ^y =b  f was
^y =b
 f was increased from 0.500 to 0.790, showing that obtained in this study for the lignin nanofiber yarn
the yarn strength was less than the tensile strength of with the twist factor of 125; this was very uncommon
the constituent fibers. With the increase of the lateral for the classical yarn, but could happen in the theoret-
pressure, the fragmentation process occurred more ical study. The reasons for this high ratio could be the
prominently, and lc was decreased due to the increase higher values of nanofiber aspect ratio, the fiber specific
of the yarn strain (Figure 8). Decreasing to nanoscale volume and the twist value of nanofiber yarns. These
length had a major effect on increasing the yarn could lead to higher lateral pressure in yarn, thereby
strength. As shown in Figure 9, the estimated yarn affecting fiber interaction; especially, for brittle fibers
strength could be increased to 189.550 MPa when lc such as lignin, this could lead to the smaller value of
was decreased to 213.950 nm. Although there were no lc, as compared with the conventional fibers.45 These
experimental results for the lignin nanofiber twisted indicated that the nanofiber yarn strength could have
yarn strength to verify the theoretical strength, we been more than that of the constituent fibers if the well
could compare with the Polyacrylonitrile (PAN)- aligned nanofiber had been provided and the fragmen-
based nanofiber twisted yarn strength ranging from tation process had been fully accomplished.
1952 Textile Research Journal 88(17)

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