A Novel Technology to Improve

Strength and Service Life of

Natural Fiber Composites
Seminar by

RANJITH

Introduction
Natural Fiber Composites (NFCs) are materials in which at least
the reinforcing fibers are derived from renewable and carbon
dioxide neutral resources such as wood or plants.
Automotive & Construction: largest segments among natural fiber
composite applications. The market size for natural fiber
composites is projected to reach $5.83 billion by the year 2019.
Major challenges for natural fibers composite industry is natural
fiber quality, sensitive to humidity, not suitable for applications
requiring optimal strength.
Performance improvement in materials will drive growth for
natural fiber composites in new application areas.

Door Panel

Seat Back

Package Tray

Roof sheet

Fence

Corrugated Panel

Z-Axis Reinforcement
Wet-Flocking Technology
All laminated composite materials suffer from service life limiting
delamination failure.
This poor inter-laminar shear strength stems from lack of Zdirection inter-ply fiber reinforcement.
Traditional methods to impart the Z-direction inter-ply fiber
reinforcement (multi-directional knitting, 3-D weaving or stitching
and Z pinning) are not cost-effective.
University of Massachusetts at Dartmouth (UMD) developed a
novel Z-axis fiber reinforced resin laminar composite materials
processing technique.

Working Principle
This technique involves the electro-static pre-placement of
perpendicularly oriented short fibers between the plies during
a composites fabrication/lay-up stage.
Short fiber placement is accomplished by electro-statically
propelling short fiber elements at an uncured polymer (fluid)
matrix coated fibrous ply layer of the composite.
This electrostatic fiber coating process is called flocking.

Electro-static Flocking unit

Experimental Work
To characterize the influence of
Surface treatments
Reinforcement architecture
Applied through-thickness microfiber reinforcement
on the delamination resistance of jute fiber/epoxy laminated
composite materials.

Tensile and in-plane shear tests were also conducted to gain a

more holistic understanding of the effect of through-thickness
reinforcement on mechanical properties.

Materials
Reinforcement
Plain weave jute fabric with areal weight of 330 g/m2
Unidirectional jute yarn pre-forms with a linear density of 1440 tex
Matrix material
Two part Epoxy resin system 2000/2120 series amine-cure with hardener to resin
mass ratio of 27:100
Materials for Fiber Surface Treatment
Sodium Hydroxide pellets (NaOH), acetic acid,
3-Triethoxysilylpropylamine (APTES), phenolphthalein indicator
Dow Corning Z-6173 silane coupling agent
Flock fiber for Z-axis reinforcement
Nylon fibers 3-denier, 1.3 mm length

Fiber Surface Treatment

Alkali Treatment:
Jute fabrics and preforms were soaked for 2 hours in a 5% (w/w)
aqueous NaOH alkali solution then rinsed with distilled water and
soaked in a 2% aqueous acetic acid solution for an additional 1 hour.
Neutrality of the fabrics and pre-forms was verified using a
phenolphthalein solution followed by thorough rinsing with distilled
water and drying at 80C overnight.
This treatment swells the amorphous regions of the fibers and
removes approximately 41% of the hemicellulose.
This has the effect of fibrillating the jute structure & increases its
effective surface area giving more area for the epoxy matrix to
penetrate and adhere to.

Silane Treatment:
A solution of 1% Dow Corning Z-6173 silane agent in methanol
was prepared.
Alkali treated, jute fabrics and preforms were soaked in the
prepared silane treatment solution for 1 h. Two silane agents were
used and compared: APTES and Dow Corning Z-6173.
This treatment aims to increase the affinity of the cellulosic parts
of the jute fibers with the epoxy matrix by grafting coupling
agents onto the cellulose chain.
Efficacy of treatments was confirmed using Fourier Transform
Infrared Spectroscopy (FTIR) performed on a Digilab Excalibur
FTS 3000MX spectrometer.

Natural Fiber Composite Panel Fabrication

The desired number of 260 mm 260 mm plies cut from the fabric
roll were laid up in a [0/90]n sequence and pre-compacted in a
hydraulic press.
The vacuum infusion procedure was adopted for NFC panel
fabrication.
For Z-axis inter-ply reinforcement, nylon flock fibers were applied
to the individual laminate plies using wet-flocking technology.
After which the laminate were laid up and infused with resin
following the standard vacuum infusion procedure.

Double Cantilever Beam Testing

To introduce the initial crack, a thin Teflon film is inserted in the
mid-plane of the laminar panel stack during the fabrication of the
composite.
The test coupons were cut to the desired dimensions according to
ASTM D5528.
Piano hinges were adhered to the ends of the delaminated arms
using a quick-set epoxy.
In The final step sample preparation was to apply measured tick
marks on the sample sides by first applying correction fluid and
then marking every 1 mm for the first 25 mm past the initial
delamination with black ink.

Reinforcement

Z-axis flock fibers

Thickness (mm)

No

11.0 (0.08)

Yes

15.0 (0.09)

No

7.08 (0.07)

Yes

11.6 (0.13)

Silane-treated plain weave

Silane-treated unidirectional

Table 1: Details of the fabricated NFC panels

Standard Double Cantilever Beam

(DCB) Specimen with Piano hinges

Double Cantilever Beam (DCB) Test samples

Results and Discussion

Surface Treatment
The purpose was to remove impurity and hemicellulose on the
fiber surface and to impart chemical accessibility to hydroxyl
group of cellulose to promote silane coupling agent reactivity.
The average percentage weight loss for alkali treated jute yarns,
was found to be (11 1.7)%
FTIR analysis of the alkali treated yarns showed a loss of peaks
at 1735 and 1240 cm-1 implies that a portion of the
hemicelluloses was removed by this treatment.
This finding supports the successful partial removal of
hemicellulose and other impurities.

 FTIR analysis of the silane treated yarns showed that a similar

spectral peak near 1100 cm-1 for yarns treated with APTES and Z6173.

Peaks near 1100 cm-1 wavenumber indicate that SiOC bonds

are formed, which suggests that the silane coupling agent reacted
to cellulose hydroxyl groups.

This implies that the agent has chemically coupled itself to the
fiber structure rather than simply being physically adhered to the
surface.

FTIR spectra of
raw and alkali-treated
jute fiber

FTIR spectra of APTES

and Dow Corning
Z- 6173 treated
jute fiber.

Mechanical Performance Properties

For both types of reinforcement architecture, fiber surface
treatment increased fracture toughness.
Z-axis inter-laminar reinforcement fibers had a profound positive
effect on the fracture toughness of laminated composites for both
pre-form architectures tested in this study.
The addition of this reinforcement increased fracture initiation
toughness by 81% for plain weave reinforcement, and 65% for
unidirectional reinforcement.
These dramatic increases in fracture toughness are as a result of
energy consumed by the flock fiber pull-out and fiber
breaking.This required an additional amount of energy to
overcome for crack growth, thereby increasing fracture toughness.

Change in fracture
toughness by flock
based Z-axis fiber
inter-ply reinforcement

Scanning electron
microscope (SEM)
images of DCB
fracture surfaces

 It is important to examine its effect on other in-plane

mechanical properties to obtain a more holistic view of the
effect of this type of reinforcement.
For both plain weave and unidirectional reinforcement
architectures, tensile strength and modulus experience losses
with the addition of Z-axis reinforcement.

Effect of Z-axis reinforcement on (a) Youngs modulus and (b) Tensile strength

 A comparison plot of the ILSS of silane-treated composites with

and without Z-axis flock reinforcement.
Interestingly, ILSS is seen to increase by 13% and 18% for plain
weave and unidirectional reinforcement, respectively.
This increase is a result of flocking fibers crossing the plane of
shearing, thus providing additional resistance to that loading.

Effect of flock
reinforcement on ILSS.

Specific Modulus Comparison

One of the major advantages of natural plant-based fibers is their
low density, and high specific properties.
To examine how these materials would compete in todays
composite material market, it is important to evaluate the strength
properties of natural fiber composites on a per unit mass basis.
Therefore to explore the potential of structural application of
NFCs, the specific moduli of jute fiber/epoxy composites in this
study were compared with that of glass/epoxy composites.
The values for specific modulus of glass fiber/epoxy composites
were taken from literature available.

 Surface treated plain weave jute/epoxy composites have a 28%

greater specific modulus than plain weave glass/epoxy
composites.
Specific modulus of surface treated UD jute/epoxy composites is
only 10% lower than that of UD glass/epoxy composites.

Specific modulus of jute fiber and glass fiber reinforced epoxy composites.

Conclusions
This study explored the influence of surface treatments,
reinforcement architecture, and applied through-thickness microfiber
reinforcement on the interlaminar fracture toughness of jute
fiber/epoxy laminated composite materials.
During this process, the following conclusions were made:
A combination of alkali and silane grafting surface treatments
increased delamination resistance of jute/epoxy composites by
10% due to an increased interfacial bond strength.
The use of University of Massachusetts Dartmouths patented Zaxis reinforcement wet-flocking technology was successfully
extended to the vacuum infusion method, thereby increasing its
applicability.

 Through-thickness microfiber reinforcement greatly improved the

delamination resistance of these composites (81% plain weave,
65% unidirectional), but degraded in-plane tensile properties by a
small value due to the introduction of resin rich layers with nonaligned reinforcing fibers.
Through-thickness reinforcement also improved ILSS by 13% and
16% for plain weave and unidirectional reinforcement,
respectively, as the reinforcing fibers bridged the plane under shear
loading.
This shows that on stiffness per unit mass basis, the composites
produced in this study can compete with more traditional glassfiber reinforced composites. Coupling this with the increased
sustainability and low energy of production of the jute fibers makes
them a very attractive choice for polymer composite reinforcement.

REFERENCES
Pinto M, Chalivendra V, Kim Y, Lewis A, Evaluation of
surface treatment and fabrication methods for jute fiber/epoxy
laminar composites, Polym Compos- 2014
M. Pinto, V.B. Chalivendra, Y.K. Kim, A.F. Lewis, Improving
the strength and service life of jute/epoxy laminar composites
for structural applications, College of Engineering,
University of Massachusetts Dartmouth, Massachusetts, USA2015.