Moisture Absorption Effects on the Mechanical Properties of Epoxy

Nano Composites.
1
Azharuddin Kazi*and 2 E Suresh
1,2
Dept. of Mechanical Engineering
P E S School of Engineering, Hosur Road, Bangalore 560 100, India

ABSTRACT

Plasticcompositematerialhasbeenintofrontierofresearchasoneofthenewcompetitive
materials in engineering. Especially, fiber reinforced plastic (FRPs) is a relatively new class of
compositematerialmanufacturedfromfibersandresins,andhasprovenefficientandeconomicalfor
thedevelopmentandrepairofnewanddeterioratingstructures.Inthiswork,wereporttheeffectof
moistureonthemechanical propertiesofepoxycompositesstrengthenedwithMWNTs.Different
compositionofcarbonnanotubes(MWNT)(0.10.2%)weremixedwithepoxymatrixbysonication
methodandcastingswerepreparedbymouldingtechnique.Thedifferentmechanicalpropertieswere
evaluated at room temperature. One set ofsamples were immersed indistilledwater at 50C for
moistureabsorptionandstrengthdegradationstudies.Themoistureabsorptiondataoneachspecimen
istabulated and analyzed for the absorption characteristics. From the moisture absorption curves,
maximummoisturecontentanddiffusioncoefficientswerecalculatedforallthesamples.Thewet
mechanicalpropertiesimportantforthetechnologicalapplicationsweregeneratedincludingfracture
toughness,flexuralstrengthandmodulus.Also,thespecimensweretestedforthedegradationstudies
aftertheabsorptionofmaximummoisture.Inadditiontotheaboveinvestigations,thehardnessofthe
resultingnanocompositeswasalsochecked.Allthestudieswerecarriedouttocharacterizeneatresin
castingsoftheresinsystemunderstudywithandwithoutcarbonnanotubesandthusgeneratesome
dataonvariouspropertiesasmentionedabove.Howeverthereisalotofscopeforfutureworkonneat
resincastingsandaswellasatlaminatelevelonthesenanocompositestooptimizethesecomposites
forpracticalaerospaceapplicationsespeciallyforthefuselageoftheairflights.

.
Author for Correspondence
*[email protected]
[email protected]
 Nomenclature

S= Tensile Strength CB=concentration of moisture

E= Modulus of Elasticity
V= Volume Fraction at the boundaries of the
f= Fiber specimen.
m= Matrix DC= diffusion coefficient.
c= Composite G=dimensionless absorption
Ef= Youngs modulus of
Parameter.
fibre
Vf= Volume fraction of h=thickness of the composite specimen under
fibre Consideration.
Em= Youngs modulus of matrix Mt=moisture content at any timet.
Vm= Volume fraction of matrix Mm=moisture content upon
W = Weight of moist specimen
saturation.
Wd =Weight of dry specimen
t=time of exposure of the specimen to
C=concentration of moisture in the test environment.
specimen. ln(Dct/h2)=dimensionless diffusion
Ci=concentration of moisture at parameter.
any time i.

Introduction
Following the technological developments deteriorating structures. The mechanical
industries are searching for lighter weight, properties of FRPs make them ideal for
higher strength and safer material to meet the widespread applications in various industries
demands of structural designs and for worldwide. The enhancement of the
economic benefit. In order to extend the mechanical and structural properties due to
application area of plastics, plastic composites addition of fibers makes FRPs ideal materials
are developed by adding reinforcement for aircraft parts, aerospace structures, and
materials to the polymer matrix. Some of the railways, marine and other industrial
reinforcements used in structural and industrial applications [1]
applications are Carbon, Aramid and Glass
fibers the most commonly used is glass fiber. Experimental Details
Plastic composite material has therefore The main aim of this chapter is to present an
become one of the new competitive materials overall picture as to how the studies related to
in engineering. Fiber reinforced plastic is a this project were conducted.This chapter
relatively new class of composite material includes detailed descriptions on Neat Resin
manufactured from fibers and resins, and has Castings with and without nano fillers (CNT),
proven efficient and economical for the the experimental setup used, the procedures
development and repair of new and adopted during the conduct of studies related
to this project, the moisture absorption studies casting should get released easily from the
and mechanical properties of both wet and dry mould different types of releasing agents has
castings. been used out of which Frekote 770-NC was
more advantageous compared to PVA (Poly
Preparation of Neat Resin Casting: This is Vinyl Alcohol) in releasing the casting easily
the first stage of the experimental process. The from the mould 7Insert spacer (Based on the
neat epoxy resin castings were prepared using thickness of casting) of the required
materials such as Epoxy resin, Amine hardener dimensions between the two mould plates and
and Diluent seal the sides of the mould with silicon sealant.
Calculations for Resin Hardener System: Clamp the sides of the mould with C- clamps.
Density of epoxy Resin: 1.2 g/cc Now remove the two beakers from the vacuum
Matrix ratio (Resin + Hardner): 100:12 oven mix the hardner with the resin and stir it
Volume of the mould (cc): 25cmX25cmX0.3 in a stirrer for 5mins and pour into the mould.
cm Now allow the mould for 24hours at room
Weight = Density x volume temperature and then for post curing in
Total Weight (resin + hardener) required = temperature oven at 50C/1/2hr, 70/1hr and
density of resin X volume of the mould 85/2hrs.
=1.2 X 250 X 250 X 3 = 225grams
Mix ratio for the epoxy system (LY556 + Equipments Used for the preparation of
HY951) is 100:12 Neat Resin Castings
i.e., Resin required = (100/112) x 225 = 1.Vacuumovenusedfordegassingtheepoxy
200gms resinSystem
Similarly Hardener required = (12/112) x 225
= 24.10gms
Procedure for preparing Neat Resin
Casting:
1
Two beakers were taken and washed with
acetone and keep it for some time so that it
dries.As per the ratio of resin and hardner that
is 100:12 the weight of resin and hardener
was calculated. 2Weigh the resin in one beaker
and hardener in other beaker Mix the resin
with 10ml of diluent K77 (which reduces the
viscosity of resin) thoroughly .3Place the two Fig: Vacuum Oven
beakers in the vacuum oven for degassing so
that the moisture in the resin and hardener 2. UltraSonicatorusedforevenlydispersing
vanishes to get a clear Neat resin casting with nanoparticlesinliquids
no air bubbles 4Both the beakers should be in
the vacuum oven till it is completely degassed
and a continues monitoring is required so that
the resin does not come out of the beakers.
5
Now clean the two mould plates with acetone
apply Frekote FMS (Mould Sealer) on to the
surface of the mould with brush so that the
finished surface having small pores gets
vanished. 6After some time apply Frekote
770-NC (Mould releasing agent) so that the
 Fig: Ultra Sonicator
3. Post curing was done to verify that the
castings are completely cured

Fig: Castings with MWCNT

Cutting of specimens using water jet cutting

machine:
After the castings are prepared, cutting of the
specimens was done as per the standard
dimensions
Fig: Post curing oven
Casting Produced

Fig: Neat Resin casting

Preparation of Casting with Multi Walled
Carbon Nano Tubes (MWCNT): Fig: Water jet Cutting Machine
Matrix System: Epoxy Resin (LY556) &
Amine Hardener (HY951)
Diluent: K77
Carbon Nano Tubes: MWCNT (Purity > 98
%, Length=1-5 microns & Diameter= 6 20
nm)
Solvent: Ethanol

Fig: Sample Specimens for Testing

Testing of Mechanical Properties:

 2 2
h M 2 M 1
Dc
4 M m t2 t1

Where
M 2 M 1 Slope

t2 t1
Mechanical strength degradation studies were
carried out after the specimens absorbed
maximum moisture content percentage
degradation was calculated using the equation
given as

% degradation =
Fig: Universal Testing Machine
The mechanical properties (Fracture
toughness, Flexural strength and modulus) of
the dry specimens (with and without CNT)
were determined using universal testing
machine (INSTRON)

Moisture Absorption Studies:

To study the moisture absorption behavior,
specimens were placed in a constant
temperature distilled water bath maintained at
50C after taking its initial dry weights. The Fig: Specimens in constant water temperature
specimens were periodically taken out from bath
the water bath to measure their weight gain as Results and Discussions
outlined below The specimens were first taken This section deals with the tabulation of the
out of the bath and were placed on a filter results obtained from the experimental studies,
paper. Each specimen was wiped with the filter and has been further divided into sub sections
paper to remove the free moisture adhering to devoted to results from experimental studies
its surfaces as well as the edges. Then the related to mechanical properties, moisture
wiped specimens were weighed on an absorption and strength degradation studies.
electronic balance and immediatel returned to
the water bath. This was done in order to The dry mechanical properties (flexural
minimize any possible loss of moisture from strength and modulus, fracture toughness) of
the specimen at room temperature conditions. neat resin casting (NRC) and nano composites
The percentage moisture gain by the specimen are shown in the tables below
was calculated by the equation as follows
(W Wd )
M 100
Wd
Diffusion and degradation Studies:
The diffusion coefficient Dc for each specimen
was calculated using the equation given as
 Material Flexural Flexural Flexural Flexural
Strength Strength modulus Modulus
(kg/mm) (N) (kg/mm) (N)
Neat Resin 12.12 118.89 420.12 4.12x103
Casting
NRC with 0.1% 11.45 112.32 354.17 3.47x103
MWCNT
NRC with 0.2% 13.80 135.37 432.8 4.24x103
MWCNT
Table 1.1 Flexural strength and modulus of NRC and nanocomposites
From the table, it is observed that both flexural strength and modulus of nano composite
(0.2%MWCNT) were increased significantly as compared to neat resin casting and casting with
0.1%MWCNT. This is due to poor interfacial bonding b/w the nanotubes and epoxy matrix in case of
0.1%.

Material Fracture Toughness (Mpa

m)
Neat Resin Casting 4.505

NRC with 0.1% 3.649

MWCNT
NRC with 0.2% 3.103
MWCNT
Table 1.2 Fracture toughness of NRC and nanocomposites
From the table, it is observed that fracture toughness of nano composite is less than that of neat resin
casting. This is due to poor dispersion of nanotubes in the epoxy matrix.

Material Time Sqrt time Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Average
and (hrs) (hrs)
Percentage
Moisture
gain fot
NRC 1896 43.54 2.53 2.596 2.647 2.583 2.666 2.604

0.1% 1896 43.54 2.384 2.371 2.388 2.451 2.424 2.404

MWCNT
0.2% 1536 39.19 2.171 2.165 2.160 2.158 2.155 2.161
MWCNT
Table 1.3 Percentage Moisture gain for NRC and casting with 0.1% MWCNT 0.2% MWCNT
From the above table it is observed that by increasing the percentage of MWCNT the moisture
absorptionis decreased.
Calculation of Diffusion parameters

Sl.No Material %Mm Dc 10-7(mm2/sec) Time of exposure

(Days)
1. Neat Resin Casting 2.60 4.793 10-7 64
2. NRC with 0.1% 2.40 5.408 10-7 64
MWCNT
3. NRC with 0.2% 2.16 7.968 10-7 64
MWCNT
Table 1.4: Difussion Parameters of NRC and Nano Composites

Degradation studies
The absorption of moisture will reduce the strength of the composite. The wet mechanical
properties of neat resin casting with 0.2% carbon nano tubes are represented.

Flexural Strength (kg/mm) Flexural Modulus (kg/mm)

Dry Wet % Dry Wet %

Degradation Degradation

Average 13.61 10.30 24.45 444.4 432.8 5.818

Table 1.5: Degradation of Flexural strength and modulus of nanocomposites

Sl No Fracture Toughness (Mpa m) % Degradation

Dry Wet
Average 3.10 2.302 25.80
Table 1.6: Degradation of Fracture toughness of nanocomposites
From the above table, it is seen that the fracture toughness degradation is more compare to flexural
strength degradation and is around 26%.

Conclusion Epoxy matrix is modified with multi walled

carbon nanotubes. Castings were prepared and mechanical and morphological properties of
properties were evaluated and tabulated. The Nano composites, Vol.2, No.2 Page 45-51
time consumed was more to freeze the correct (2008) 7887
method for the preparation of the castings with [5] Qiang Lu1 and Baidurya Bhattacharya2
and without nano fillers. From this, it can be Department of Mechanical Engineering,
concluded that some of the properties were Northwestern University, Evanston, IL 60208,
significantly changed with the addition of USA (2006)
nanotubes. [6]T K SINDHU, R SARATHI* Department
of Aerospace Engineering, Indian Institute of
Mechanical properties like Flexural strength Technology April 2007
and modulus were increased with 0.2% [7] Smith and Lowry, Polymeric Composites
nanotubes, as compared to lower CNT Laboratory, University of Washington
concentration. Fracture toughness values were
not changed significantly with the nanotube
inclusions due to poor dispersion of nanotubes
in the epoxy matrix (FESEM images) and also
nanotubes in the composite could not take up
the full load longituidinal direction for the
same reason. Moisture absorption (Mm) values
are 2.6% for neat resin casting and 2.1% for
nanocomposites. Moisture absorption (Mm)
values decrease with increase in CNT
concentration. Diffusion Coefficient (Dc)
values increase with increase in CNT
concentration. Degradation of flexural strength
and modulus are around 24% and 5.8%,
fracture toughness degradation will be 26%.
Properties were not changed significantly for
addition of lower concentration of nanotubes,
Addition of still higher concentration of
nanotubes may give significant changes in the
properties.

References
[1] Autar K. Kaw (2005). Composite Materials
(2nd ed.) Page 234-240 (2007)
[2] Matzkanin, George A.; Yolken, H. Thomas,
Evaluation of Polymer matrix
composites(vol1) Page 32-46
[3] Tong, L, A.P. Mouritz, and M.k. Bannister.
3D Fibre Reinforced Polymer Composites
Oxford Elsevier, Page 12-54 (2002

[4]S. Y. Lee1*, I. A. Kang Thermal,