Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

6
7/21/2019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber http://slidepdf.com/reader/full/investigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 1/6 DOI 10.1515/secm-2013-0292 Sci Eng Compos Mater 2014; aop Mayank Agarwal, Mohamand Arif, Ankita Bisht, Vinay K. Singh* and Sunanda Biswas Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber  Abstract: An epoxy resin (EP) matrix has been modi- fied with depolymerized natural rubber (DNR). The 0.5, 1.0, 1.5, 2.0, and 2.5 wt% DNR-filled epoxy were used for the present investigation. The primary aim of this development is to scrutinize the mechanical properties of such cured epoxy filled with DNR. When the rub- ber content was low, the mechanical strength was low and the free volume of DNR in epoxy matrix was less. With the increase in rubber content, the free volume of rubber in the composite increases and the mechanical strength increases; however, after a specific weight per- centage of rubber, if we increase the amount of rubber, the mechanical strength decreases and the free volume of rubber in the composite increases quickly, but with the increase in DNR weight percentage in epoxy matrix, the hardness decreases. The scanning electron micros- copy (SEM) results justified the results obtained from the mechanical tests. Keywords: depolymerized natural rubber; epoxy resin; mechanical properties. *Corresponding author: Vinay K. Singh, College of Technology, G.B. Pant University of Agriculture and Technology, Pantnagar-263 145, Uttarakhand, India, e-mail: [email protected] Mayank Agarwal, Mohamand Arif, Ankita Bisht and Sunanda Biswas: College of Technology, G.B. Pant University of Agriculture and Technology, Pantnagar-263 145, Uttarakhand, India 1 Introduction Epoxy resins (EP) are used in a variety of applications because they are a very important class of thermoset- ting polymers that exhibit high tensile strength, excel- lent chemical and corrosion resistance, good thermal stability, low density and low creep, and reasonable performance at elevated temperature. Hence, they are widely used in structural adhesives, surface coatings, and electrical laminates and as matrix resins for reinforced composite materials. However, general epoxy systems usually suffer the shortage of toughness due to the high levels of cross-linking, which can and usually does result in brittle behavior. Liquid rubber can be used as a tough- ing material for EP because it is normally derived from synthetic rubber. During the polymerization, the rubber phase separates because it becomes less miscible with the epoxy matrix, forming a sludge of rubber that is dis- persed in the EP matrix. Several methods have been pro- posed to increase the toughness of EP by the addition of rubber in uncured EP and then controlling the polymeri- zation reactions in order to restrict the phase separation [1–6]. The rubbery materials that are added to the uncured epoxy are types of copolymers with variable acrylonitrile contents. The studies reported that, to modify EP, mostly modified liquid rubber was used, such as liquid rubber modified by divinylbenzene (DVB), hydroxyl terminated butadiene (HTPB), carboxyl terminated butadiene-acry- lonitrile (CTBN), or isocyanate terminated polybutadi- ene (NCOPBER) [4, 7–9]. However, due to the increasing awareness of environmental issues, natural latex rubber has attracted great interest because it is a renewable resource. In the present study, natural rubber latex is used as a toughing material for EP. The properties of modified epoxy are studied by tensile test. The dispersion of rubber in the matrix of epoxy is verified by the scanning electron microscopy (SEM) test. 2 Materials and methods 2.1 Epoxy resin The bisphenol A-type EP (CY230) used for this study was purchased from M/s Petro Araldite Pvt. Ltd. (Chennai, India). Epoxy (CY230) is widely used in indus- trial application because of its high strength and good mechanical adhesiveness. It is also a good solvent and has good chemical resistance over a wide range of temperature. Bereitgestellt von | De Gruyter / TCS Angemeldet | 10 248 254 158 Heruntergeladen am | 01 09 14 10:32

description

This research paper is related with the subject of Epoxy Resin

Transcript of Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

Page 1: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

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DOI 101515secm-2013-0292 Sci Eng Compos Mater 2014 aop

Mayank Agarwal Mohamand Arif Ankita Bisht Vinay K Singh and Sunanda Biswas

Investigation of toughening behavior of epoxyresin by reinforcement of depolymerized latex

rubber

Abstract An epoxy resin (EP) matrix has been modi-

fied with depolymerized natural rubber (DNR) The 05

10 15 20 and 25 wt DNR-filled epoxy were used

for the present investigation The primary aim of this

development is to scrutinize the mechanical properties

of such cured epoxy filled with DNR When the rub-

ber content was low the mechanical strength was low

and the free volume of DNR in epoxy matrix was less

With the increase in rubber content the free volume ofrubber in the composite increases and the mechanical

strength increases however after a specific weight per-

centage of rubber if we increase the amount of rubber

the mechanical strength decreases and the free volume

of rubber in the composite increases quickly but with

the increase in DNR weight percentage in epoxy matrix

the hardness decreases The scanning electron micros-

copy (SEM) results justified the results obtained from

the mechanical tests

Keywords depolymerized natural rubber epoxy resin

mechanical properties

Corresponding author Vinay K Singh College of Technology GB

Pant University of Agriculture and Technology Pantnagar-263 145

Uttarakhand India e-mail vks2319yahoocoin

Mayank Agarwal Mohamand Arif Ankita Bisht and Sunanda

Biswas College of Technology GB Pant University of Agriculture

and Technology Pantnagar-263 145 Uttarakhand India

1 IntroductionEpoxy resins (EP) are used in a variety of applications

because they are a very important class of thermoset-

ting polymers that exhibit high tensile strength excel-

lent chemical and corrosion resistance good thermal

stability low density and low creep and reasonable

performance at elevated temperature Hence they are

widely used in structural adhesives surface coatings and

electrical laminates and as matrix resins for reinforced

composite materials However general epoxy systems

usually suffer the shortage of toughness due to the high

levels of cross-linking which can and usually does result

in brittle behavior Liquid rubber can be used as a tough-

ing material for EP because it is normally derived from

synthetic rubber During the polymerization the rubber

phase separates because it becomes less miscible with

the epoxy matrix forming a sludge of rubber that is dis-

persed in the EP matrix Several methods have been pro-posed to increase the toughness of EP by the addition of

rubber in uncured EP and then controlling the polymeri-

zation reactions in order to restrict the phase separation

[1ndash6] The rubbery materials that are added to the uncured

epoxy are types of copolymers with variable acrylonitrile

contents The studies reported that to modify EP mostly

modified liquid rubber was used such as liquid rubber

modified by divinylbenzene (DVB) hydroxyl terminated

butadiene (HTPB) carboxyl terminated butadiene-acry-

lonitrile (CTBN) or isocyanate terminated polybutadi-

ene (NCOPBER) [4 7ndash9] However due to the increasing

awareness of environmental issues natural latex rubber

has attracted great interest because it is a renewable

resource In the present study natural rubber latex is used

as a toughing material for EP The properties of modified

epoxy are studied by tensile test The dispersion of rubber

in the matrix of epoxy is verified by the scanning electron

microscopy (SEM) test

2 Materials and methods

21 Epoxy resin

The bisphenol A-type EP (CY230) used for this study

was purchased from Ms Petro Araldite Pvt Ltd

(Chennai India) Epoxy (CY230) is widely used in indus-

trial application because of its high strength and good

mechanical adhesiveness It is also a good solvent and

has good chemical resistance over a wide range of

temperature

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7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 26

2 M Agarwal et al Investigation of toughening behavior of epoxy resin

22 Hardener HY951

The hardener HY951 purchased from Ms Petro Araldite Pvt

Ltd was used as a curing agent In the present investigation

9 wt has been used in all materials developed The weight

percentage of hardener used in the present investigation is

as per the recommendation of Singh and Gope [10]

23 Natural rubber latex

Natural rubber latex (NR) was purchased from Ms Allied

Business (Pantnagar India) It has 60 dry rubber content

The NR has outstanding flexibility and high mechanical

strength Moreover it is a renewable resource whereas its

synthetic counterparts are mostly manufactured from non-

renewable oil-based resources Therefore NR has created

a high level of interest regarding its use and its derivatives

24 Preparation of the material

241 Depolymerization of NR

Depolymerization means opening the active linkage in the

polymer backbone by the reaction of a reagent with reactive

polar group Depolymerization can reduce the chain length

of natural rubber In general a depolymerized natural

rubber (DNR) can be obtained by mastication photolysis

chemical decomposition or the like of the natural rubber

Mastication is a method for accelerating reduction in the

molecular weight by breaking the rubber molecular chains

of the raw rubber through a mechanical action and heating

in a roller mill or internal mixer and then adding a peptiz-

ing agent such as a mercaptan [11] Vitaly and Eduardo [12]

used the photolysis method for breaking the molecular

chains with light energy that is ultraviolet light Another

approach that has been used to reduce the molecular

weight of natural rubber is chemical decomposition This

method is the degradation of molecular chains by chemical

reagents In 1996 Tanaka et al [13] proposed the process fordepolymerizing natural rubber which comprised adding

a carbonyl compound to natural rubber latex or depro-

teinized natural rubber and then subjecting the resulting

natural rubber or deproteinized natural rubber to air oxida-

tion in the presence of a radical-forming agent The results

showed that the DNR having a narrow molecular weight

distribution can be obtained at high reaction efficiency

In the present method 60 total dry content natural

rubber latex was diluted by distilled water to a concen-

tration of 5 wt based on rubber content followed by the

Table 1 Compositions of cured epoxy filled with DNR

Designation of

composition

EP (CY983090983091983088)

(wt)

Hardener (HY983097983093983089)

(wt)

DNR

(wt)

C983088 983089983088983088 983097 983088983088

C983089 983089983088983088 983097 983088983093

C983090 983089983088983088 983097 983089983088

C983091 983089983088983088 983097 983089983093

C983092 983089983088983088 983097 983090983088

C983093 983089983088983088 983097 983090983093

addition of CH3 CH

2 COCH

3 and K

2 S

2 O

8 in an amount of 4ndash6

vol of total volume and 2 wt based on the rubber content

respectively The pH of latex was adjusted to about 9ndash10 with

10 wt aqueous KOH solution Then the reaction mixture

was mechanically stirred at a speed of 200ndash300 rpm at 60deg C

on the sand (for the equal distribution of heat) for 24 h in

the presence of air At the end of the reaction the reaction

mixture was coagulated by 1 wt aqueous CaCl2 solution

The coagulated substance was dissolved in n -hexane and

stirred with magnetic bar for 12 h Then the resulting solu-

tion was allowed to stand overnight and filtered The filtrate

mixture was bathed with methanol followed by vacuum

drying at 40deg C until the weight is made constant

242 Preparation of rubber-filled EP

The DNR was dissolved completely in EP (CY230) at 100deg Cusing a mechanical stirrer at a speed of 500 rpm for 2 h After

2 h the whole solution is taken out and allowed to cool to a

temperature of 80deg C When a temperature of 80deg C has been

attained a 9 wt hardener is mixed immediately After the

addition of the hardener viscous solution was again mixed

mechanically by a high-speed mechanical stirrer The

viscous solution so obtained is poured into different moulds

for sample preparation for tensile testing The compositions

of cured epoxy filled with DNR are given in Table 1

3 Results

31 Characterization of cured epoxy filledwith DNR

The specimens were gold coated and examined by SEM

using a LEO435V6 instrument The accelerating voltage

was kept at 10 kV and magnification factor of times250 The

SEM test was conducted on the fractured surface to see the

mechanism of the fracture The state of dispersion of DNR

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M Agarwal et al Investigation of toughening behavior of epoxy resin 3

A B

C D

Figure 1 SEM images of fracture surface for several cured epoxy (A) pure epoxy (B) 05 wt rubber (C) 10 wt rubber (D) 15 wt rubber

into the resin matrix plays a significant role on the improve-

ment of the mechanical properties of the cured epoxy It is

seen from Figure 1AndashD that DNR are well dispersed in the EP

matrix and sharp surface failure occurs in all the tests The

absence of any voids indicates a good adhesion between

the DNR and epoxy matrix Figure 1AndashC shows that the DNR

added to the epoxy matrix has completely bonded with it

and there is no free volume of DNR in the epoxy matrix

From Figure 1D it is evident that there is some free volume

of DNR that has not chemically bonded with the matrix as

estimated from the observations Due to this reason the

mechanical strength increases up to 1 wt rubber and then

decreases with further increase in the weight percentage of

rubber due to the excess or free volume of rubber

32 Mechanical properties

The tensile test specimen (Figure 2) prepared for each

weight percentage of DNR was loaded in uniaxial tension

on a 100 kN servohydraulic universal testing machine

(ADMET Norwood MA USA) at 01 mms crosshead speed

according to ISO 16081972 The standard gauge length of

the specimen should be given by L0 =565radicA

0 where A

0

is the cross-sectional area of specimen (m2 ) and L0 is the

standard gauge length of the specimen (m)

From the stress strain curves as shown in Figure 3

the ultimate strength modulus of elasticity and percent

elongations were determined The room temperature and

humidity during testing were 32deg C and 88 respectively

Remarkable differences have been observed in the stress

strain behavior due to the addition of DNR in the EP matrix

33 Tensile properties

From the results remarkable differences can be seen on

the ultimate tensile strength of DNR-filled cured epoxy

having different weight percentages of DNR tested at

01 mms crosshead speeds given in Table 2 It can be seen

from the results that for all specimens containing 10 wtDNR the ultimate tensile strength is highest from among

the other compositions reported About 42 increase in

ultimate tensile strength due to the addition of 10 wt

DNR has been noticed compared to pure epoxy This

increase in strength is observed due to the intermolecular

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7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

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4 M Agarwal et al Investigation of toughening behavior of epoxy resin

Grip section

Gage

length

Width of

grip section

Dia or width

ldquoReducedrdquo section

Figure 2 Specimen of tension test

80

70

60

50

40

S t r e s s ( M P a )

30

20

10

00 002 004 006 008 010

0 wt of R

10 wt of R

20 wt of R

15 wt of R

25 wt of R

05 wt of R

012 014

Strain

Figure 3 Stress strain curve of different weight percentages of DNR

Table 2 Tensile properties of cured epoxy filled with different weight percentages of DNR

Designation of

composition

DNR (wt) Ultimate

strength (MPa)

Elongation () Toughness

(MPa)

Modulus of

elasticity (MPa)

C983088 983088983088 983092983095983092983088 983093983089983088 983089983095983091983095 983089983096983096983097983090983096

C983089 983088983093 983093983090983090983096 983097983093983088 983091983088983088983089 983089983088983094983095983095983091

C983090 983089983088 983094983095983091983091 983089983090983093983096 983093983090983090983097 983097983089983090983095983092

C983091 983089983093 983092983089983091983088 983089983089983088983088 983090983097983093983094 983094983095983089983095983094

C983092 983090983088 983091983097983096983097 983095983089983095 983089983092983089983094 983093983090983094983095983093

C983093 983090983093 983091983093983090983094 983094983096983088 983089983090983090983094 983093983089983091983096983097

1480

13

12

11

10

9

8

7

6

5

4

U l t i m a t e s t r e

n g t h ( M P a )

70

60

50

40

0

30

2005 10 15 2520

Ultimate strength (MPa)

Elongation

E l o n g a t i o n ( )

Rubber (wt)

Figure 4 Mechanical properties of cured epoxy filled with different

weight percentages of DNR

bonding between the rubber particle to the resin particles

A further addition of DNR on the EP decreases the ulti-

mate tensile strength of the DNR-filled cured epoxy due

to excess rubber particles which is present free withoutbonding Similar observations have been noticed for

percent elongation as shown in Figure 4 About 247 times

increase in the modulus of elasticity has been observed

due to the addition of 10 wt DNR at 01 mms crosshead

speed A further addition of the DNR decreases the percent

elongation but is higher than the neat epoxy material

About 14 times increase in the modulus of elasticity is

noticed for the 20 wt DNR-filled cured epoxy

The variation of the modulus of elasticity and tough-

ness with the variation of rubber weight percentage is

as shown in Figure 5 In Figure 5 it is seen that a non-

linear relation exists between the modulus of elasticity

and weight percentage of filler materials The maximum

modulus of elasticity is found for neat resin It has been

noticed that toughness is found to be maximum at the

addition of 10 wt DNR compared to pure epoxy This

increase in strength is due to the proper intermolecular

bonding between rubber particle to the resin particles A

further addition of DNR on the EP decreases the tough-

ness of the DNR-filled cured epoxy due to excess rubber

particles which is present unbonded Keeping in view the

importance of the modulus of elasticity and toughness in

design and analysis an attempt has been made to model

an empirical relation of the following type to interpret the

filler polymer interaction

Up to 10 wt DNR

2 2

R RET=1101 (W ) -2014 (W )+1087 R =1 (1)

More than 10 wt DNR

2 2

R RET=-1951 (W ) +9725 (W )-7924 R =1

(2)

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M Agarwal et al Investigation of toughening behavior of epoxy resin 5

where E and T are the modulus of elasticity in MPa and

toughness in MPa respectively WR denotes the weight

percentage of DNR In the present case toughness behav-

ior is the opposite after the addition of more than 1 wt

DNR

34 Hardness

All hardness tests are conducted on a Rockwell hardness

testing machine supplied by PSI Pvt Ltd (New Delhi

India) on R scale The effect of the weight percentage of

DNR on the hardness values of DNR-filled cured epoxy is

shown in Figure 6 It is found that the hardness of neat EP

is 44 HRR The hardnesses of the fabricated cured epoxy

filled with 05 10 15 20 and 25 wt DNR are 43 41 39

37 and 36 HRR respectively as given in Table 3

Figure 6 indicates that the hardness decreases with

the DNR content reflecting the reinforcement formed in

the DNR-filled cured epoxy The variation of the ratio of

the modulus of elasticity with the hardness of DNR-filled

cured epoxy is shown in Figure 7 Figure 7 illustrates that

the hardness value follows a nonlinear relation with themodulus of elasticity of the DNR-filled cured epoxy An

attempt has been made to correlate the modulus of elas-

ticity with hardness The following correlation has been

obtained

5 4 3

R R R

2 2

R R

EH=-6950 (W ) +4976 (W ) -1298 (W )

+1518 (W ) -8544 (W )+4293 R =1

(3)

where E and H are the modulus of elasticity in MPa and

hardness in R-scale respectively WR denotes the weight

6

5

4

3

2

1

0

M o d u l u s o f e l a s t i c i t y ( M P a )

2000

1800

1600

1400

1200

1000

800

600

4000 05 10 15 2520

Modulus of elasticity

Toughness

T o u g h n e

s s ( M P a )

Rubber (wt)

Figure 5 Modulus of elasticity and toughness of cured epoxy filled

with different weight percentages of DNR

H a r d n

e s s ( H R R )

45

44

43

42

41

40

39

38

37

36

350 05 10 15 2520

Rubber (wt)

Figure 6 Hardness of cured epoxy filled with different weight

percentages of DNR

Table 3 Hardness of cured epoxy filled with different weightpercentages of DNR

Designation of

composition

DNR (wt) Hardness

C983088 983088983088 983092983092

C983089 983088983093 983092983091

C983090 983089983088 983092983089

C983091 983089983093 983091983097

C983092 983090983088 983091983095

C983093 983090983093 983091983094

M o d u l u s o f e l a s t i c i t y ( M P a ) h a r d n e s s ( H R R )

45

50

35

40

25

30

15

20

5

0

10

0 05 10 15 2520

Rubber (wt)

EH

Poly (EH)

Figure 7 EH ratio of cured epoxy filled with different weight

percentages of DNR

percentage of DNR Equation (3) indicates that the non-

linear relationship between the modulus of elasticity

and hardness has a good correlation It shows that the

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6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

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Page 2: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 26

2 M Agarwal et al Investigation of toughening behavior of epoxy resin

22 Hardener HY951

The hardener HY951 purchased from Ms Petro Araldite Pvt

Ltd was used as a curing agent In the present investigation

9 wt has been used in all materials developed The weight

percentage of hardener used in the present investigation is

as per the recommendation of Singh and Gope [10]

23 Natural rubber latex

Natural rubber latex (NR) was purchased from Ms Allied

Business (Pantnagar India) It has 60 dry rubber content

The NR has outstanding flexibility and high mechanical

strength Moreover it is a renewable resource whereas its

synthetic counterparts are mostly manufactured from non-

renewable oil-based resources Therefore NR has created

a high level of interest regarding its use and its derivatives

24 Preparation of the material

241 Depolymerization of NR

Depolymerization means opening the active linkage in the

polymer backbone by the reaction of a reagent with reactive

polar group Depolymerization can reduce the chain length

of natural rubber In general a depolymerized natural

rubber (DNR) can be obtained by mastication photolysis

chemical decomposition or the like of the natural rubber

Mastication is a method for accelerating reduction in the

molecular weight by breaking the rubber molecular chains

of the raw rubber through a mechanical action and heating

in a roller mill or internal mixer and then adding a peptiz-

ing agent such as a mercaptan [11] Vitaly and Eduardo [12]

used the photolysis method for breaking the molecular

chains with light energy that is ultraviolet light Another

approach that has been used to reduce the molecular

weight of natural rubber is chemical decomposition This

method is the degradation of molecular chains by chemical

reagents In 1996 Tanaka et al [13] proposed the process fordepolymerizing natural rubber which comprised adding

a carbonyl compound to natural rubber latex or depro-

teinized natural rubber and then subjecting the resulting

natural rubber or deproteinized natural rubber to air oxida-

tion in the presence of a radical-forming agent The results

showed that the DNR having a narrow molecular weight

distribution can be obtained at high reaction efficiency

In the present method 60 total dry content natural

rubber latex was diluted by distilled water to a concen-

tration of 5 wt based on rubber content followed by the

Table 1 Compositions of cured epoxy filled with DNR

Designation of

composition

EP (CY983090983091983088)

(wt)

Hardener (HY983097983093983089)

(wt)

DNR

(wt)

C983088 983089983088983088 983097 983088983088

C983089 983089983088983088 983097 983088983093

C983090 983089983088983088 983097 983089983088

C983091 983089983088983088 983097 983089983093

C983092 983089983088983088 983097 983090983088

C983093 983089983088983088 983097 983090983093

addition of CH3 CH

2 COCH

3 and K

2 S

2 O

8 in an amount of 4ndash6

vol of total volume and 2 wt based on the rubber content

respectively The pH of latex was adjusted to about 9ndash10 with

10 wt aqueous KOH solution Then the reaction mixture

was mechanically stirred at a speed of 200ndash300 rpm at 60deg C

on the sand (for the equal distribution of heat) for 24 h in

the presence of air At the end of the reaction the reaction

mixture was coagulated by 1 wt aqueous CaCl2 solution

The coagulated substance was dissolved in n -hexane and

stirred with magnetic bar for 12 h Then the resulting solu-

tion was allowed to stand overnight and filtered The filtrate

mixture was bathed with methanol followed by vacuum

drying at 40deg C until the weight is made constant

242 Preparation of rubber-filled EP

The DNR was dissolved completely in EP (CY230) at 100deg Cusing a mechanical stirrer at a speed of 500 rpm for 2 h After

2 h the whole solution is taken out and allowed to cool to a

temperature of 80deg C When a temperature of 80deg C has been

attained a 9 wt hardener is mixed immediately After the

addition of the hardener viscous solution was again mixed

mechanically by a high-speed mechanical stirrer The

viscous solution so obtained is poured into different moulds

for sample preparation for tensile testing The compositions

of cured epoxy filled with DNR are given in Table 1

3 Results

31 Characterization of cured epoxy filledwith DNR

The specimens were gold coated and examined by SEM

using a LEO435V6 instrument The accelerating voltage

was kept at 10 kV and magnification factor of times250 The

SEM test was conducted on the fractured surface to see the

mechanism of the fracture The state of dispersion of DNR

Bereitgestellt von | De Gruyter TCS

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7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

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M Agarwal et al Investigation of toughening behavior of epoxy resin 3

A B

C D

Figure 1 SEM images of fracture surface for several cured epoxy (A) pure epoxy (B) 05 wt rubber (C) 10 wt rubber (D) 15 wt rubber

into the resin matrix plays a significant role on the improve-

ment of the mechanical properties of the cured epoxy It is

seen from Figure 1AndashD that DNR are well dispersed in the EP

matrix and sharp surface failure occurs in all the tests The

absence of any voids indicates a good adhesion between

the DNR and epoxy matrix Figure 1AndashC shows that the DNR

added to the epoxy matrix has completely bonded with it

and there is no free volume of DNR in the epoxy matrix

From Figure 1D it is evident that there is some free volume

of DNR that has not chemically bonded with the matrix as

estimated from the observations Due to this reason the

mechanical strength increases up to 1 wt rubber and then

decreases with further increase in the weight percentage of

rubber due to the excess or free volume of rubber

32 Mechanical properties

The tensile test specimen (Figure 2) prepared for each

weight percentage of DNR was loaded in uniaxial tension

on a 100 kN servohydraulic universal testing machine

(ADMET Norwood MA USA) at 01 mms crosshead speed

according to ISO 16081972 The standard gauge length of

the specimen should be given by L0 =565radicA

0 where A

0

is the cross-sectional area of specimen (m2 ) and L0 is the

standard gauge length of the specimen (m)

From the stress strain curves as shown in Figure 3

the ultimate strength modulus of elasticity and percent

elongations were determined The room temperature and

humidity during testing were 32deg C and 88 respectively

Remarkable differences have been observed in the stress

strain behavior due to the addition of DNR in the EP matrix

33 Tensile properties

From the results remarkable differences can be seen on

the ultimate tensile strength of DNR-filled cured epoxy

having different weight percentages of DNR tested at

01 mms crosshead speeds given in Table 2 It can be seen

from the results that for all specimens containing 10 wtDNR the ultimate tensile strength is highest from among

the other compositions reported About 42 increase in

ultimate tensile strength due to the addition of 10 wt

DNR has been noticed compared to pure epoxy This

increase in strength is observed due to the intermolecular

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Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

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4 M Agarwal et al Investigation of toughening behavior of epoxy resin

Grip section

Gage

length

Width of

grip section

Dia or width

ldquoReducedrdquo section

Figure 2 Specimen of tension test

80

70

60

50

40

S t r e s s ( M P a )

30

20

10

00 002 004 006 008 010

0 wt of R

10 wt of R

20 wt of R

15 wt of R

25 wt of R

05 wt of R

012 014

Strain

Figure 3 Stress strain curve of different weight percentages of DNR

Table 2 Tensile properties of cured epoxy filled with different weight percentages of DNR

Designation of

composition

DNR (wt) Ultimate

strength (MPa)

Elongation () Toughness

(MPa)

Modulus of

elasticity (MPa)

C983088 983088983088 983092983095983092983088 983093983089983088 983089983095983091983095 983089983096983096983097983090983096

C983089 983088983093 983093983090983090983096 983097983093983088 983091983088983088983089 983089983088983094983095983095983091

C983090 983089983088 983094983095983091983091 983089983090983093983096 983093983090983090983097 983097983089983090983095983092

C983091 983089983093 983092983089983091983088 983089983089983088983088 983090983097983093983094 983094983095983089983095983094

C983092 983090983088 983091983097983096983097 983095983089983095 983089983092983089983094 983093983090983094983095983093

C983093 983090983093 983091983093983090983094 983094983096983088 983089983090983090983094 983093983089983091983096983097

1480

13

12

11

10

9

8

7

6

5

4

U l t i m a t e s t r e

n g t h ( M P a )

70

60

50

40

0

30

2005 10 15 2520

Ultimate strength (MPa)

Elongation

E l o n g a t i o n ( )

Rubber (wt)

Figure 4 Mechanical properties of cured epoxy filled with different

weight percentages of DNR

bonding between the rubber particle to the resin particles

A further addition of DNR on the EP decreases the ulti-

mate tensile strength of the DNR-filled cured epoxy due

to excess rubber particles which is present free withoutbonding Similar observations have been noticed for

percent elongation as shown in Figure 4 About 247 times

increase in the modulus of elasticity has been observed

due to the addition of 10 wt DNR at 01 mms crosshead

speed A further addition of the DNR decreases the percent

elongation but is higher than the neat epoxy material

About 14 times increase in the modulus of elasticity is

noticed for the 20 wt DNR-filled cured epoxy

The variation of the modulus of elasticity and tough-

ness with the variation of rubber weight percentage is

as shown in Figure 5 In Figure 5 it is seen that a non-

linear relation exists between the modulus of elasticity

and weight percentage of filler materials The maximum

modulus of elasticity is found for neat resin It has been

noticed that toughness is found to be maximum at the

addition of 10 wt DNR compared to pure epoxy This

increase in strength is due to the proper intermolecular

bonding between rubber particle to the resin particles A

further addition of DNR on the EP decreases the tough-

ness of the DNR-filled cured epoxy due to excess rubber

particles which is present unbonded Keeping in view the

importance of the modulus of elasticity and toughness in

design and analysis an attempt has been made to model

an empirical relation of the following type to interpret the

filler polymer interaction

Up to 10 wt DNR

2 2

R RET=1101 (W ) -2014 (W )+1087 R =1 (1)

More than 10 wt DNR

2 2

R RET=-1951 (W ) +9725 (W )-7924 R =1

(2)

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Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 56

M Agarwal et al Investigation of toughening behavior of epoxy resin 5

where E and T are the modulus of elasticity in MPa and

toughness in MPa respectively WR denotes the weight

percentage of DNR In the present case toughness behav-

ior is the opposite after the addition of more than 1 wt

DNR

34 Hardness

All hardness tests are conducted on a Rockwell hardness

testing machine supplied by PSI Pvt Ltd (New Delhi

India) on R scale The effect of the weight percentage of

DNR on the hardness values of DNR-filled cured epoxy is

shown in Figure 6 It is found that the hardness of neat EP

is 44 HRR The hardnesses of the fabricated cured epoxy

filled with 05 10 15 20 and 25 wt DNR are 43 41 39

37 and 36 HRR respectively as given in Table 3

Figure 6 indicates that the hardness decreases with

the DNR content reflecting the reinforcement formed in

the DNR-filled cured epoxy The variation of the ratio of

the modulus of elasticity with the hardness of DNR-filled

cured epoxy is shown in Figure 7 Figure 7 illustrates that

the hardness value follows a nonlinear relation with themodulus of elasticity of the DNR-filled cured epoxy An

attempt has been made to correlate the modulus of elas-

ticity with hardness The following correlation has been

obtained

5 4 3

R R R

2 2

R R

EH=-6950 (W ) +4976 (W ) -1298 (W )

+1518 (W ) -8544 (W )+4293 R =1

(3)

where E and H are the modulus of elasticity in MPa and

hardness in R-scale respectively WR denotes the weight

6

5

4

3

2

1

0

M o d u l u s o f e l a s t i c i t y ( M P a )

2000

1800

1600

1400

1200

1000

800

600

4000 05 10 15 2520

Modulus of elasticity

Toughness

T o u g h n e

s s ( M P a )

Rubber (wt)

Figure 5 Modulus of elasticity and toughness of cured epoxy filled

with different weight percentages of DNR

H a r d n

e s s ( H R R )

45

44

43

42

41

40

39

38

37

36

350 05 10 15 2520

Rubber (wt)

Figure 6 Hardness of cured epoxy filled with different weight

percentages of DNR

Table 3 Hardness of cured epoxy filled with different weightpercentages of DNR

Designation of

composition

DNR (wt) Hardness

C983088 983088983088 983092983092

C983089 983088983093 983092983091

C983090 983089983088 983092983089

C983091 983089983093 983091983097

C983092 983090983088 983091983095

C983093 983090983093 983091983094

M o d u l u s o f e l a s t i c i t y ( M P a ) h a r d n e s s ( H R R )

45

50

35

40

25

30

15

20

5

0

10

0 05 10 15 2520

Rubber (wt)

EH

Poly (EH)

Figure 7 EH ratio of cured epoxy filled with different weight

percentages of DNR

percentage of DNR Equation (3) indicates that the non-

linear relationship between the modulus of elasticity

and hardness has a good correlation It shows that the

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 66

6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Page 3: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 36

M Agarwal et al Investigation of toughening behavior of epoxy resin 3

A B

C D

Figure 1 SEM images of fracture surface for several cured epoxy (A) pure epoxy (B) 05 wt rubber (C) 10 wt rubber (D) 15 wt rubber

into the resin matrix plays a significant role on the improve-

ment of the mechanical properties of the cured epoxy It is

seen from Figure 1AndashD that DNR are well dispersed in the EP

matrix and sharp surface failure occurs in all the tests The

absence of any voids indicates a good adhesion between

the DNR and epoxy matrix Figure 1AndashC shows that the DNR

added to the epoxy matrix has completely bonded with it

and there is no free volume of DNR in the epoxy matrix

From Figure 1D it is evident that there is some free volume

of DNR that has not chemically bonded with the matrix as

estimated from the observations Due to this reason the

mechanical strength increases up to 1 wt rubber and then

decreases with further increase in the weight percentage of

rubber due to the excess or free volume of rubber

32 Mechanical properties

The tensile test specimen (Figure 2) prepared for each

weight percentage of DNR was loaded in uniaxial tension

on a 100 kN servohydraulic universal testing machine

(ADMET Norwood MA USA) at 01 mms crosshead speed

according to ISO 16081972 The standard gauge length of

the specimen should be given by L0 =565radicA

0 where A

0

is the cross-sectional area of specimen (m2 ) and L0 is the

standard gauge length of the specimen (m)

From the stress strain curves as shown in Figure 3

the ultimate strength modulus of elasticity and percent

elongations were determined The room temperature and

humidity during testing were 32deg C and 88 respectively

Remarkable differences have been observed in the stress

strain behavior due to the addition of DNR in the EP matrix

33 Tensile properties

From the results remarkable differences can be seen on

the ultimate tensile strength of DNR-filled cured epoxy

having different weight percentages of DNR tested at

01 mms crosshead speeds given in Table 2 It can be seen

from the results that for all specimens containing 10 wtDNR the ultimate tensile strength is highest from among

the other compositions reported About 42 increase in

ultimate tensile strength due to the addition of 10 wt

DNR has been noticed compared to pure epoxy This

increase in strength is observed due to the intermolecular

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 46

4 M Agarwal et al Investigation of toughening behavior of epoxy resin

Grip section

Gage

length

Width of

grip section

Dia or width

ldquoReducedrdquo section

Figure 2 Specimen of tension test

80

70

60

50

40

S t r e s s ( M P a )

30

20

10

00 002 004 006 008 010

0 wt of R

10 wt of R

20 wt of R

15 wt of R

25 wt of R

05 wt of R

012 014

Strain

Figure 3 Stress strain curve of different weight percentages of DNR

Table 2 Tensile properties of cured epoxy filled with different weight percentages of DNR

Designation of

composition

DNR (wt) Ultimate

strength (MPa)

Elongation () Toughness

(MPa)

Modulus of

elasticity (MPa)

C983088 983088983088 983092983095983092983088 983093983089983088 983089983095983091983095 983089983096983096983097983090983096

C983089 983088983093 983093983090983090983096 983097983093983088 983091983088983088983089 983089983088983094983095983095983091

C983090 983089983088 983094983095983091983091 983089983090983093983096 983093983090983090983097 983097983089983090983095983092

C983091 983089983093 983092983089983091983088 983089983089983088983088 983090983097983093983094 983094983095983089983095983094

C983092 983090983088 983091983097983096983097 983095983089983095 983089983092983089983094 983093983090983094983095983093

C983093 983090983093 983091983093983090983094 983094983096983088 983089983090983090983094 983093983089983091983096983097

1480

13

12

11

10

9

8

7

6

5

4

U l t i m a t e s t r e

n g t h ( M P a )

70

60

50

40

0

30

2005 10 15 2520

Ultimate strength (MPa)

Elongation

E l o n g a t i o n ( )

Rubber (wt)

Figure 4 Mechanical properties of cured epoxy filled with different

weight percentages of DNR

bonding between the rubber particle to the resin particles

A further addition of DNR on the EP decreases the ulti-

mate tensile strength of the DNR-filled cured epoxy due

to excess rubber particles which is present free withoutbonding Similar observations have been noticed for

percent elongation as shown in Figure 4 About 247 times

increase in the modulus of elasticity has been observed

due to the addition of 10 wt DNR at 01 mms crosshead

speed A further addition of the DNR decreases the percent

elongation but is higher than the neat epoxy material

About 14 times increase in the modulus of elasticity is

noticed for the 20 wt DNR-filled cured epoxy

The variation of the modulus of elasticity and tough-

ness with the variation of rubber weight percentage is

as shown in Figure 5 In Figure 5 it is seen that a non-

linear relation exists between the modulus of elasticity

and weight percentage of filler materials The maximum

modulus of elasticity is found for neat resin It has been

noticed that toughness is found to be maximum at the

addition of 10 wt DNR compared to pure epoxy This

increase in strength is due to the proper intermolecular

bonding between rubber particle to the resin particles A

further addition of DNR on the EP decreases the tough-

ness of the DNR-filled cured epoxy due to excess rubber

particles which is present unbonded Keeping in view the

importance of the modulus of elasticity and toughness in

design and analysis an attempt has been made to model

an empirical relation of the following type to interpret the

filler polymer interaction

Up to 10 wt DNR

2 2

R RET=1101 (W ) -2014 (W )+1087 R =1 (1)

More than 10 wt DNR

2 2

R RET=-1951 (W ) +9725 (W )-7924 R =1

(2)

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 56

M Agarwal et al Investigation of toughening behavior of epoxy resin 5

where E and T are the modulus of elasticity in MPa and

toughness in MPa respectively WR denotes the weight

percentage of DNR In the present case toughness behav-

ior is the opposite after the addition of more than 1 wt

DNR

34 Hardness

All hardness tests are conducted on a Rockwell hardness

testing machine supplied by PSI Pvt Ltd (New Delhi

India) on R scale The effect of the weight percentage of

DNR on the hardness values of DNR-filled cured epoxy is

shown in Figure 6 It is found that the hardness of neat EP

is 44 HRR The hardnesses of the fabricated cured epoxy

filled with 05 10 15 20 and 25 wt DNR are 43 41 39

37 and 36 HRR respectively as given in Table 3

Figure 6 indicates that the hardness decreases with

the DNR content reflecting the reinforcement formed in

the DNR-filled cured epoxy The variation of the ratio of

the modulus of elasticity with the hardness of DNR-filled

cured epoxy is shown in Figure 7 Figure 7 illustrates that

the hardness value follows a nonlinear relation with themodulus of elasticity of the DNR-filled cured epoxy An

attempt has been made to correlate the modulus of elas-

ticity with hardness The following correlation has been

obtained

5 4 3

R R R

2 2

R R

EH=-6950 (W ) +4976 (W ) -1298 (W )

+1518 (W ) -8544 (W )+4293 R =1

(3)

where E and H are the modulus of elasticity in MPa and

hardness in R-scale respectively WR denotes the weight

6

5

4

3

2

1

0

M o d u l u s o f e l a s t i c i t y ( M P a )

2000

1800

1600

1400

1200

1000

800

600

4000 05 10 15 2520

Modulus of elasticity

Toughness

T o u g h n e

s s ( M P a )

Rubber (wt)

Figure 5 Modulus of elasticity and toughness of cured epoxy filled

with different weight percentages of DNR

H a r d n

e s s ( H R R )

45

44

43

42

41

40

39

38

37

36

350 05 10 15 2520

Rubber (wt)

Figure 6 Hardness of cured epoxy filled with different weight

percentages of DNR

Table 3 Hardness of cured epoxy filled with different weightpercentages of DNR

Designation of

composition

DNR (wt) Hardness

C983088 983088983088 983092983092

C983089 983088983093 983092983091

C983090 983089983088 983092983089

C983091 983089983093 983091983097

C983092 983090983088 983091983095

C983093 983090983093 983091983094

M o d u l u s o f e l a s t i c i t y ( M P a ) h a r d n e s s ( H R R )

45

50

35

40

25

30

15

20

5

0

10

0 05 10 15 2520

Rubber (wt)

EH

Poly (EH)

Figure 7 EH ratio of cured epoxy filled with different weight

percentages of DNR

percentage of DNR Equation (3) indicates that the non-

linear relationship between the modulus of elasticity

and hardness has a good correlation It shows that the

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 66

6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Page 4: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 46

4 M Agarwal et al Investigation of toughening behavior of epoxy resin

Grip section

Gage

length

Width of

grip section

Dia or width

ldquoReducedrdquo section

Figure 2 Specimen of tension test

80

70

60

50

40

S t r e s s ( M P a )

30

20

10

00 002 004 006 008 010

0 wt of R

10 wt of R

20 wt of R

15 wt of R

25 wt of R

05 wt of R

012 014

Strain

Figure 3 Stress strain curve of different weight percentages of DNR

Table 2 Tensile properties of cured epoxy filled with different weight percentages of DNR

Designation of

composition

DNR (wt) Ultimate

strength (MPa)

Elongation () Toughness

(MPa)

Modulus of

elasticity (MPa)

C983088 983088983088 983092983095983092983088 983093983089983088 983089983095983091983095 983089983096983096983097983090983096

C983089 983088983093 983093983090983090983096 983097983093983088 983091983088983088983089 983089983088983094983095983095983091

C983090 983089983088 983094983095983091983091 983089983090983093983096 983093983090983090983097 983097983089983090983095983092

C983091 983089983093 983092983089983091983088 983089983089983088983088 983090983097983093983094 983094983095983089983095983094

C983092 983090983088 983091983097983096983097 983095983089983095 983089983092983089983094 983093983090983094983095983093

C983093 983090983093 983091983093983090983094 983094983096983088 983089983090983090983094 983093983089983091983096983097

1480

13

12

11

10

9

8

7

6

5

4

U l t i m a t e s t r e

n g t h ( M P a )

70

60

50

40

0

30

2005 10 15 2520

Ultimate strength (MPa)

Elongation

E l o n g a t i o n ( )

Rubber (wt)

Figure 4 Mechanical properties of cured epoxy filled with different

weight percentages of DNR

bonding between the rubber particle to the resin particles

A further addition of DNR on the EP decreases the ulti-

mate tensile strength of the DNR-filled cured epoxy due

to excess rubber particles which is present free withoutbonding Similar observations have been noticed for

percent elongation as shown in Figure 4 About 247 times

increase in the modulus of elasticity has been observed

due to the addition of 10 wt DNR at 01 mms crosshead

speed A further addition of the DNR decreases the percent

elongation but is higher than the neat epoxy material

About 14 times increase in the modulus of elasticity is

noticed for the 20 wt DNR-filled cured epoxy

The variation of the modulus of elasticity and tough-

ness with the variation of rubber weight percentage is

as shown in Figure 5 In Figure 5 it is seen that a non-

linear relation exists between the modulus of elasticity

and weight percentage of filler materials The maximum

modulus of elasticity is found for neat resin It has been

noticed that toughness is found to be maximum at the

addition of 10 wt DNR compared to pure epoxy This

increase in strength is due to the proper intermolecular

bonding between rubber particle to the resin particles A

further addition of DNR on the EP decreases the tough-

ness of the DNR-filled cured epoxy due to excess rubber

particles which is present unbonded Keeping in view the

importance of the modulus of elasticity and toughness in

design and analysis an attempt has been made to model

an empirical relation of the following type to interpret the

filler polymer interaction

Up to 10 wt DNR

2 2

R RET=1101 (W ) -2014 (W )+1087 R =1 (1)

More than 10 wt DNR

2 2

R RET=-1951 (W ) +9725 (W )-7924 R =1

(2)

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7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 56

M Agarwal et al Investigation of toughening behavior of epoxy resin 5

where E and T are the modulus of elasticity in MPa and

toughness in MPa respectively WR denotes the weight

percentage of DNR In the present case toughness behav-

ior is the opposite after the addition of more than 1 wt

DNR

34 Hardness

All hardness tests are conducted on a Rockwell hardness

testing machine supplied by PSI Pvt Ltd (New Delhi

India) on R scale The effect of the weight percentage of

DNR on the hardness values of DNR-filled cured epoxy is

shown in Figure 6 It is found that the hardness of neat EP

is 44 HRR The hardnesses of the fabricated cured epoxy

filled with 05 10 15 20 and 25 wt DNR are 43 41 39

37 and 36 HRR respectively as given in Table 3

Figure 6 indicates that the hardness decreases with

the DNR content reflecting the reinforcement formed in

the DNR-filled cured epoxy The variation of the ratio of

the modulus of elasticity with the hardness of DNR-filled

cured epoxy is shown in Figure 7 Figure 7 illustrates that

the hardness value follows a nonlinear relation with themodulus of elasticity of the DNR-filled cured epoxy An

attempt has been made to correlate the modulus of elas-

ticity with hardness The following correlation has been

obtained

5 4 3

R R R

2 2

R R

EH=-6950 (W ) +4976 (W ) -1298 (W )

+1518 (W ) -8544 (W )+4293 R =1

(3)

where E and H are the modulus of elasticity in MPa and

hardness in R-scale respectively WR denotes the weight

6

5

4

3

2

1

0

M o d u l u s o f e l a s t i c i t y ( M P a )

2000

1800

1600

1400

1200

1000

800

600

4000 05 10 15 2520

Modulus of elasticity

Toughness

T o u g h n e

s s ( M P a )

Rubber (wt)

Figure 5 Modulus of elasticity and toughness of cured epoxy filled

with different weight percentages of DNR

H a r d n

e s s ( H R R )

45

44

43

42

41

40

39

38

37

36

350 05 10 15 2520

Rubber (wt)

Figure 6 Hardness of cured epoxy filled with different weight

percentages of DNR

Table 3 Hardness of cured epoxy filled with different weightpercentages of DNR

Designation of

composition

DNR (wt) Hardness

C983088 983088983088 983092983092

C983089 983088983093 983092983091

C983090 983089983088 983092983089

C983091 983089983093 983091983097

C983092 983090983088 983091983095

C983093 983090983093 983091983094

M o d u l u s o f e l a s t i c i t y ( M P a ) h a r d n e s s ( H R R )

45

50

35

40

25

30

15

20

5

0

10

0 05 10 15 2520

Rubber (wt)

EH

Poly (EH)

Figure 7 EH ratio of cured epoxy filled with different weight

percentages of DNR

percentage of DNR Equation (3) indicates that the non-

linear relationship between the modulus of elasticity

and hardness has a good correlation It shows that the

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 66

6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Page 5: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 56

M Agarwal et al Investigation of toughening behavior of epoxy resin 5

where E and T are the modulus of elasticity in MPa and

toughness in MPa respectively WR denotes the weight

percentage of DNR In the present case toughness behav-

ior is the opposite after the addition of more than 1 wt

DNR

34 Hardness

All hardness tests are conducted on a Rockwell hardness

testing machine supplied by PSI Pvt Ltd (New Delhi

India) on R scale The effect of the weight percentage of

DNR on the hardness values of DNR-filled cured epoxy is

shown in Figure 6 It is found that the hardness of neat EP

is 44 HRR The hardnesses of the fabricated cured epoxy

filled with 05 10 15 20 and 25 wt DNR are 43 41 39

37 and 36 HRR respectively as given in Table 3

Figure 6 indicates that the hardness decreases with

the DNR content reflecting the reinforcement formed in

the DNR-filled cured epoxy The variation of the ratio of

the modulus of elasticity with the hardness of DNR-filled

cured epoxy is shown in Figure 7 Figure 7 illustrates that

the hardness value follows a nonlinear relation with themodulus of elasticity of the DNR-filled cured epoxy An

attempt has been made to correlate the modulus of elas-

ticity with hardness The following correlation has been

obtained

5 4 3

R R R

2 2

R R

EH=-6950 (W ) +4976 (W ) -1298 (W )

+1518 (W ) -8544 (W )+4293 R =1

(3)

where E and H are the modulus of elasticity in MPa and

hardness in R-scale respectively WR denotes the weight

6

5

4

3

2

1

0

M o d u l u s o f e l a s t i c i t y ( M P a )

2000

1800

1600

1400

1200

1000

800

600

4000 05 10 15 2520

Modulus of elasticity

Toughness

T o u g h n e

s s ( M P a )

Rubber (wt)

Figure 5 Modulus of elasticity and toughness of cured epoxy filled

with different weight percentages of DNR

H a r d n

e s s ( H R R )

45

44

43

42

41

40

39

38

37

36

350 05 10 15 2520

Rubber (wt)

Figure 6 Hardness of cured epoxy filled with different weight

percentages of DNR

Table 3 Hardness of cured epoxy filled with different weightpercentages of DNR

Designation of

composition

DNR (wt) Hardness

C983088 983088983088 983092983092

C983089 983088983093 983092983091

C983090 983089983088 983092983089

C983091 983089983093 983091983097

C983092 983090983088 983091983095

C983093 983090983093 983091983094

M o d u l u s o f e l a s t i c i t y ( M P a ) h a r d n e s s ( H R R )

45

50

35

40

25

30

15

20

5

0

10

0 05 10 15 2520

Rubber (wt)

EH

Poly (EH)

Figure 7 EH ratio of cured epoxy filled with different weight

percentages of DNR

percentage of DNR Equation (3) indicates that the non-

linear relationship between the modulus of elasticity

and hardness has a good correlation It shows that the

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Heruntergeladen am | 01 09 14 1032

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 66

6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158

Page 6: Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

7212019 Investigation of toughening behavior of epoxy resin by reinforcement of depolymerized latex rubber

httpslidepdfcomreaderfullinvestigation-of-toughening-behavior-of-epoxy-resin-by-reinforcement-of-depolymerized 66

6 M Agarwal et al Investigation of toughening behavior of epoxy resin

modulus of elasticity is directly related to the hardness of

this type of cured epoxy filled with DNR

4 Conclusions

A DNR-filled cured epoxy was prepared Such DNR-filled

cured epoxy was experimentally characterized by means

of microscopy tensile testing and hardness testing

Remarkable improvements in the mechanical proper-

ties have been noticed due to the addition of DNR in

EP Regression models were developed to simulate the

mechanical behavior of such materials from the volume

content of the DNR

Acknowledgment The authors express their gratitude

and sincere thanks to Department of Science amp Technol-

ogy India for providing finance to carry out this research

work smoothly

Received November 17 2013 accepted December 14 2013

References

[1] Huang J Kinloch AJ J Mater Sci 1992 27 2753ndash2762

[2] Huang J Kinloch AJ J Mater Sci 1992 27 2763ndash2769

[3] Guild FJ Kinloch AJ J Mater Sci 1995 30 1689ndash1697[4] Barcia FL Amaral TP Soares BG Polymer 2003 44

5811ndash5819

[5] Shukla SK Srivastava D Polym Sci 2006 100 1802ndash1806

[6] Chikhi N Fellahi S Bakar M Eur Polym J 2002 38

251ndash264

[7] Thomas R Ding Y He Y Yang L Moldenaers P Yang W Czigany T

Thomas S Polymer 2008 49 278ndash294

[8] Saadati P Baharvand H Rahimi A Morshedian J Iranian

Polym 2005 14 637ndash646

[9] Seluga U Kurzeja L Galina H Polym Bull 2008 60 555ndash567[10] Singh VK Gope PC J Reinforced Plast Compos 2010 29

2450ndash2468

[11] Okwu UN Akinlabi AK J Appl Polym Sci 2007 106

1291ndash1293

[12] Vitaly R Eduardo A Food Chem 2005 92 235ndash254

[13] Tanaka Y Sakaki T Kawasaki A Hayashi M Kanamaru K

Shibata K US Patent 51999856600

Bereitgestellt von | De Gruyter TCS

Angemeldet | 10 248 254 158