tensile and fracture properties of chemically treatment...

International Journal of Mechanical & Mechatronics Engineering IJMME-IJENS Vol:19 No:04 90

192804-7575-IJMME-IJENS © August 2019 IJENS I J E N S

Tensile and Fracture Properties of Chemically Treatment Date Palm

Tree Fibre Reinforced Epoxy

Mohammed Y. Abdellah1,4*, Abo-El Hagag A. Seleem2, W. W. Marzok3, A. M. Hashem1 1Mechanical Engineering Department, Faculty of Engineering, South Valley University, Qena, 83523

2Sun Miser petroleum company, Egypt 3Production Engineering and Design Department, Faculty of Engineering, Minia Universities, Minia, Egypt, 61111

4Mechanical Engineering Department, College of Engineering and Islamic Architecture, Umm Al-Qura University, Makkah,

KSA

Corresponding author: *[email protected], [email protected]

Abstract-- Composite materials reinforced using natural

fibers have great intense in the last few years, due to their

advantages to health and it is considered a friendly

environment. Nowadays, the date palm trees are attractive,

especially in the middle east region, this is due to their

widespread which make them cheap and available with a

large amount. The date palm trees are used in ancient

years in many simple industries such as ropes,

scuttle …etc. In the present study date, palm trees have

been used to reinforce epoxy resin to be used in advanced

industrial applications. Firstly, three different types of

chemical treatments are carried out on the date palm

trees; the fibers are immersion in three different types of a

chemical solution (CH3COOH, HCl, and alkaline NaOH)

with three different concentrations 10% and 20 % and

50 % at boiling temperature for 1 and 2hrs. Then, these

fibres are mechanically grinding to small chipped fibres.

These fibres are mixed with epoxy resin. The effect of

chemical treatment in the date palm trees fibres is analysis

using electro-scan microstructure (SEM) examination. The

tensile test is carried out over the standard tensile test

specimens of that composite to study the effectiveness of

reinforcement with the epoxy resin. The resistance to

fracture and to crack propagation are investigated

measuring surface release energy of each composite

specimen of date palm trees fibres reinforced epoxy

(DPTFRE). The fracture properties are measured using

standard composite compact tension test specimen at room

temperature. The maximum and minimum values of

tensile, crack resistance are measures. The results show

that HCl treatment gives good compatibility with date

palm trees fibres.

Index Term-- date palm tree, composite material, fracture

toughness, release energy.

1. INTRODUCTION

The composite materials take an excellent role in a lot of

applications, composite material which is two or more than

two materials have two phases; reinforced phase (fiber, flak or

particulates) and the matrix phase (polymer, ceramic or metal) [1]. Many works preferred natural fibre due to their

biodegradable and environment-friendly [2-5]. Natural fibres

play a competitive role and receive special consideration

compared to conventional glass and carbon fiber. The Date

palm tree fibres reinforced polymer as a composite material have been investigated in [6-8].

Alawar et al. [9] investigated the effect of different treatment

methods on DPTF. Alkaline solution treatment using NaOH

and acetic treatment of Hydrochloric acid (HCL) were carried

out with different concentrations at boiling temperatures. The

effect of these treatments on mechanical, chemical and surface

morphology was observed. The results showed that NaOH

gave good and optimum values while HCL resulted in

mechanical properties degradation.

Khanam and AlMaadeed [10] studied the fabrication and

preparation of date palm tree fibres with recycled blend polymer composites. The date palm trees were used without

chemical treatment. The adhesive between reinforcement and

matrix was achieved using compatibilizer with different %

contents. Effect of compatibilizer contents on mechanical,

thermal, morphological properties was observed and studied.

It resulted in tensile strength and hardness enhancement.

Thermal stability was gotten better and water absorption else.

Oushabi et al. [11] studied the effect of alkaline NaOH

treatment on date palm tree fibres (DPF). 5 % of wt NaOH

was used for 1hr. with different concentrations of silane agent

to increase interfacial bonding with a polymer. SEM analysis

showed a formation of silane layer on the alkaline surface of the fibre. The treatment enhanced the debonding the DPF

strength with polyurethane and epoxy.

Elbadry [12] investigated the effect of two different types of

treatments on the behaviors of DPF. The first treatment was

surface hand cleaning using soft sand cloth. The second one

was heat treatment at 100 0C for 1.5 hrs. The last treatment

was using the chemical NaOH solution for 1 hr. at 100 0C.

The results showed an observable enhancement with the three

treatment types, while their variability was less than that of

raw DPF.

Ahmadi et al. [13] used untreatable trunk fibre of date palm tree to reinforce epoxy resin as a composite material. The DPT

had get cut into three different lengths and at three different

percent volume fraction. The composite had been fabricated

using hand molding method. The results concluded that the

changing of fibre length had no observable effect on neither

tensile nor flexural properties. Increasing fibre volume

fraction did not affect or improve tensile strength while it

gives an observable improvement with bending strength.

Alsaeed et al. [14] used fibre pull out test method to measure

interfacial adhesive of DPT fibre with epoxy resin. DPT fibre

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had given treatment by NaOH alkaline solution treatment with

(0-9%) concentrations. SEM analysis investigated the surface

morphology and fibre damage. The results recommended that

optimum treatment of DPT was at 6% concentration, while 10

mm length was the optimum embedded length.

Asadzadeh et al. [15] reinforced different types of polymers

by using DPT fibre to investigate their effect on bending strength. They used five levels of fibre volume fraction, these

fibres were mixed by coupling agent to increase the

debondablity and interfacial adhesive between polymers. The

results gave enhancement in bending properties and a decrease

in breaking elongation.

AL-SULAIMAN [16] investigated the mechanical

properties, water absorption and machinability of DPT leaves

reinforced polymer composite laminates. They fabricated the

composite laminates using three different fabrication methods.

The polymer resins were phenol-formaldehyde resin and a

two-component Bisphenol resin. They observed that both tensile and flexural strength had to get enhancement, while in

Bisphenol resin gave better results. Fatigue behaviors for

Bisphenol resin had to get better. Water absorption also for

Bisphenol resin was better than phenol-formaldehyde resin.

Machinability for all composites was enhanced.

The fracture toughness of reinforced composite polymer was

studied in many works [17-19], but these studies were about

reinforced synthetic fibre, little studies were about natural

fibres, Betelie et al. [20] studied the fracture toughness of

natural fibre reinforced epoxy. They fabricated a standard

compact tension specimen which was obtained from a

composite plate manufactured using hand molding method technique. The results showed that with increasing fibre

volume fraction the fracture toughness had getting

enhancement. Natural fibres as a reinforcement phase with a

polymer matrix to create friendly environmental product were

attractive in many works [21-26].

1.2 Objective of the present study

The main goals of the present study are:

a) To investigate the effect of different chemical treatments

of both acetic and alkaline solutions on tensile properties

and fracture toughness or crack resistant.

b) It is also to study the date palm tree fibre surface

morphology using SEM micro examination under different

chemical solution and at two immersion periods.

The paper methodology is; in the first paragraph the fabricated process using molding technique is outlined and explained, the

second section the standard tensile and fracture test

summarized, the third term the SEM micro examination is

displayed then the main results are related. Finally, the

recommended conclusion is cited.

2.Material Preparation and testing

2.1 Date palm tree chemical treatment

The used materials are date palm tree fibres (see Fig. 1) that

surrounding the stems collected from Qena City at upper of

Egypt, these fibres have the physical and mechanical

properties listed in Tables 1 and 2. Firstly, the fibres get

cleaning from dust by a water bath and leave to dry in room

temperature. They manually get dismantled into bundles of

virgin fibre, then get wished again and were dried for 24 h in

room temperature as shown in Fig. (2- a). The fibre gets

chopped for small pieces using electrical mixing for 15 min

(Fig. (2-b)). The grinding fibres are then chemical treatment by three different types of solutions. The chemical treatment is

carried out to enhance the surface of natural fibre to increase

its debondablity with the polymer matrix. The interface

bonding between fibre and polymer is a dominated role in

determining the mechanical properties of natural fibre. The

fibre is immersion in three concentrations 10 %, 20 % and 50

% of the acetic solution of HCL, CH3COOH and alkaline

solution of Na OH at boiling temperature )100 oC) for 1 hr.

and 2 hr. The produced plate is nearly 3.5 mm average

thickness for all test specimens.

Table I

Physical properties of the date palm fibers with other natural types [27]

fibre types Coir Date

palm

Hemp Sisal

Density (g/cm3) 1.15–1.46

0.9–1.2 1.4–1.5

1.33–1.5

Length (mm) 20–150 20–250 5–55 900

Diameter (µm) 10–460 100–

1,000

25–

500

8–200

Specific modulus

(approx..)

4 7 40 17

Annual world

production (103)

100 4,200 214 378

Cost per weight

(USD/Kg)

0.3 0.02 1.2 1

Thermal conductivity

(W/mK)

0.047 0.083 0.115 0.07

Table II

Mechanical Properties of the date palm and other natural fibres[27]

Properties diameter Tensile

strength

(MPa)

Young’s

Modulus

(GPa)

Elongation

at break

(%)

Jute 25–200 393–773 13–26.5 1.16–1.5

Flax 10–40 600–

2,000

12–85 1–4

Sisal 50–200 468–640 9.4–22.0 3–7

Coir 100–450 131–175 4–6 15–40

Raw date

palm

fibre

100–

1,000

58–203 2–7.5 5–10

Fig. 1. Photograph of a) date palm tree b) stems surrounding by fibre c) fibres

[13, 27].



Fig. 2. a) Fibre bundles b) Fibre chopped

2.2 Sample compaction molding

The composite specimen is manufactured using compaction

molding technique. The date palm tree fibre chopped powder

is firstly mixed with epoxy resin with hardener 1:2 % each. A

thin aluminum foil is spread over the surface of lower base

and wall of the mold frame as a release agent, the steel mold

frame is 300 × 20 mm × 10 mm depth (see Fig. 3). Then the mixture paste is gradually fed and spread till the desired

thickness reach and the mold gets filed with the material past

mixture. The second step aluminum foil covers the upper

surface of the specimen paste, then a steel dummy block of 1.5

mm thick is closed the mold with very little clearance to

prevent the mold leakage. the goal of aluminum foil is to

protect the paste mixture from surface sticking. Under the

aluminum foil, a cover of leather surrounded the whole mold

to prevent leakage of epoxy. The mixed material paste is then

pressed under 3 tons load using 5 tons maximum capacity

manual hydraulic press. These conditions are chosen after many attempts to obtain the beast working parameters. The

specimen is kept under the press to consolidate and curing in

room temperature for 48 hrs. Finally, the specimens are taking

off and are ready to be cut for testing. The produced plate of

279 × 18 mm × 3 (see Fig. 3-b).

Fig. 3. Compaction molding

2.3 Mechanical testing

Standard dog-bone tensile test specimens (see Fig. 4) are cut

and are prepared on water jet machine from the specimen

previously manufactured. The tensile test is carried out using a

universal testing machine of 20 kN maximum capacity with

crosshead speed 2 mm/min according to ASTM D638-14 [28].

The load and strain are computerized measured when the

specimen is tested. The testing is carried out to full fracture of

the specimens, during the test observation of the specimen

surface damage is considered to record any change on it

during the test. Five test specimens are used for each status.

Fig. 4. schematic drawing of the tensile test specimen

2.4 Compact tension test

The fracture toughness of DPT fibres reinforced epoxy (DPTFRE) is play a dominated role in the characteristic of

materials. The fracture toughness test specimens are used

according to ASTM standard E399 [29]. Compact tension test

specimens are performed to measure the fracture toughness of

DPTFRE as shown in (Fig .5). The crack resistance has to be

measured in order to stop at the onset of degradation.

Therefore, compact tension test will investigate to obtain

satisfied fracture toughness results. The compact tension is

machined from DPTFRE accordance with the dimension

given in ASTM E399 [29] as shown in Fig.5. The initial

portion notch has to be machined with a milling cutter or with

a diamond saw and a starter crack has to be introduced at the root of the notch by tapping or sawing a fine razor blade [17-

19, 30-32]. The pre-cracked fracture specimen is loaded with

suitable loading devices. The fracture loads (PQ), obtained

from the tests of five specimens are used to determine (KIC)

values (MPa.m1/2). According to ASTM standard E399 [29],

the critical stress intensity factor for a fracture load (PQ), is

given by:

𝐊𝐈𝐂 =𝐩𝐐

𝐡√𝐰𝐟(𝐚 𝐰⁄ ) (1)

𝐆𝐈𝐂 =𝐊𝐈𝐂

2

𝐄

2

where (h) is the thickness of the specimen, (w) is the

dimension from the load line to the right-hand edge of the

specimen, as indicated in Fig. 5 and (a) is the crack length,

whose initial value (ao) is also indicated in Fig. 5. and

(𝐟(𝐚 𝐰⁄ )) is a shape correction factor



Fig. 5. Schematic drawing of compact tension test geometry

2.5 Micrographically study Micrograph study was performed by using a Scanning

Electron Microscope (SEM-EDX Philips). The examination is

performed on DPTF before and after chemical treatment.

Moreover, the cross-section of the samples was analyzed after

tensile and fracture tests to examine the fracture and bonding

between the fibre and the matrix.

3. RESULTS AND DISCUSSION 3.1 SEM micrography of treatment of DPTF

Fig. (6-a) is an electro scan microscope (SEM) photos which

illustrate that the untreatable fibres were covered by a thick

layer of impurities and a rough surface, this layer weakening

the debondability and adhesive with the resin. This layer of

contaminants which contains dust included in branches of

fibre plays a dominated role in fracture of material, as it is like

flaws in the neutral fibre [27]. These flaws decrease

debondablity between fibre and polymers. These contaminants

decrease the compatibility between fibres and polymer matrix

which means a reduction in stress transferred between the fibre and the matrix [11]. The chemical treatment of fibre

cleans the fibre surface and takes away the wax and dust. It is

causing the composite fibre bundles to change into smaller

fibre lengths. The smooth surface of the untreatable fibre is

the reason for easy fibre pull out from matrix [15, 22],

whereas, the rough-surface which is caused by chemical

treatment increases the debondiblty with the polymer matrix (

see Fig. 6 b and d), this behavior is increased in case of NaOH

treatment. The rougher surface of fibre increases with the

period of boiling in the chemical solution for 1 hr. (see Fig. 7)

The treatment using NaOH make fracture in the fibre as observed in Fig. (6-C) and Fig. (7-C).

Fig. 6. SEM photograph at 1 hr of a) Date palm tree (DPT) without treatment

b) With Hcl c) with NaOH3 d) with CH3COOH at 10 %

Fig. 7. SEM photograph at 2 hr of a) Date palm tree (DPT) without treatment

b) With Hcl c) with NaOH3 d) with CH3COOH at 10 %

3.2 Tensile test:

It is observed (Fig. 8 to Fig.10) that both treatments using

acidic media like HCL and CH3COOH, give an increase in

the strength and Young's modulus with increasing time of

treatment, while in NaOH the strength decreases, this is

attributed to that with NaOH the fibre fracture and damage

occur (Fig. 11). It is observed in Fig. 12, there is no matrix

cracking or fibre fracture for treatment with NaOH at lower

concentration 10 % for both 1 hr or 2 hrs., while, there is fibre

breaking and fibre distortion is observed at increasing

concentration 20 % for 1hr. and 2 hr. respectively (Fig. 12 c, d). Moreover, matrix damage with fibre breaking and

distortion are illustrated in the higher concentration of 50 %

(see Fig. 12 e, f). The natural fibre is highly polar respect to

NaOH [22, 33], this type of treatment increases the surface

roughness, it enables the natural fibre to remove lignin, wax,

and oils (see Fig. 12). The solution of NaOH attacks the main



construction components of the fibre and more grooves appear

on the surface of the fibre. This results in further weakening in

fibre strength, so the tensile strength starts to decrease (see

Figs. 6,7-c and Fig. 12).

The strength increases linearly with an increasing percentage

of concentration for HCL when boiling in 2 hrs. as shown in

Fig. (11-b), while the trend is nearly similar below 20 % concentration HCL after boiling in 1hr., then it decreases, this

is due to that increasing of the treatment times enhances the

surface of the fibre and make it more course and spongy (see

Figs. 6,7-b). This enhancement increases the debondablity

with the resin, therefore, it is observed in Fig.13 for 10 % and

20 % concentration of HCl boiling for 1hr, the fibre crack,

fibre tearing and breaking, this means that there is a good

adhesion occurs with the matrix while fibre fracture out of

matrix with 50 % HCl. The fibre tearing, fibre bridging,

breaking is observed which leads to effectively adhesive and

god debondablity. No matrix cracking is observed.

The Acetic acid gives the highest strength at 10 % for 1hr then

it sharply decreases, this might be attributed to the acid attack

on the fibre surface, as CH3COOH normality increases the

surface distortion [27, 34] and fibre pull out and matrix damage (see Figs. 11 and 14). This is also attributed to that

fibres tends to get closely packed owing to the removal of

hemicellulose by acetic acid treatment [34] (see Figs. 6,7-d).

All tension test data with its stander deviation are listed in

Table 3. The failure modes are net tension (see Fig. 15), there

are matrix damage and fracture near fracture surface, fibre

breakage, and distortion.

Fig. 8. Stress strain relation of DPTRE at HCl treatment at a) 10% b) 20 % c) 50 %

Fig. 9. Average Stress strain relation of DPTRE at NaOH treatment at a) 10% b) 20 % c) 50 %

Fig. 10. Average stress strain relation of DPTRE at CH3COOH treatment at a) 10% b) 20 % c) 50 %



Fig. 11. Tensile strength variation with chemical treatment concentration at a) 1hr, b) 2hr boiling temperature

Table III

Strength of Date Palm tree fiber reinforced epoxy with stander deviation

Specimens with treatments Average tensile strength (MPa) S. D Elastic Modulus, E (GPa)

(HCl 10% 1hr) 28 2.52 1.6

(HCl 10% 2hr) 41 3.34758 2.4

(HCl 20% 1hr) 53 1.52776 8.35

(HCl 20% 2hr) 62 2.52776 3.075

(HCl 50% 1hr) 43 3.52776 0.8

(HCl50% 2hr) 132 4.52776 12.1

(Acetic acid 10% 1hr) 215 2.52776 31.4

(Acetic acid 10% 2hr) 32 2.18663 3.9

(Acetic acid 20% 1hr) 61 1.02173 2.5

(Acetic acid 20% 2hr) 121 3.70016 9.01

(Acetic acid 50% 1hr) 48 2.52776 5.7

(Acetic acid 50% 2hr) 55 3.34758 1.7

(Na OH 10% 1hr) 141.6 3.32764 16

(Na OH 10% 2hr) 63 2.33073 1.5

(Na OH 20% 1hr) 123 2.52776 10.7

(Na OH 20% 2hr) 92 3.52776 5.17

(Na OH 50%1 hr) 90.5 2.79663 15.6

(Na OH 50%2 hr) 87.9 3.39262 6.34



Fig. 12. SEM photograph for NaOH treatment in composite DPTRE a) 10 %

1hr, b) 10 % 2hrs, C) 20 % 1hr., d) 20 % 2hrs, e) 50% 1hr, f) 50 % 2hr.

Fig. 13. SEM photograph for HCl treatment in composite DPTRE a) 10 %

1hr, b) 10 % 2hrs, C) 20 % 1hr., d) 20 % 2hrs, e) 50% 1hr, f) 50 % 2hr.

Fig. 14. SEM photograph for CH3COOH treatment in composite DPTRE a)

10 % 1hr, b) 10 % 2hrs,

Fig. 15. Failure Modes of some samples of tensile specimens a) HCl, b)

NaOH, c) CH3COOH for 1hr.

3.4 Fracture toughness:

Figs.16, 17 and 18 show the load-displacement curve for

treatable DPT compact tension specimen. It is clearly

demonstrated that chemical treatment has improved crack

resistance and ductility of DPT composites. The flow behavior

of the curve gives a rising in softening with nearly constant

stability, this may be due to the increase of bridging fibre at

crack face (see Fig. 20). The two-period treatment nearly

gives close results, but the failure length roughly changes as

listed in Table 4. The 5% scant of the slope gives the value of maximum load PQ at which crack is beginning to propagate.

This value is then inserted in Eqn 1, with respect to failure or

critical length of failure listed in Table 4. The fracture

toughness KIC is measured, by applying Eqn. 2 the surface

release energy is getting measured and listed in Table 4. Fig.

19 shows the measured surface release energy for all

specimens measured; it is observing the high similarity

between the results of tensile strength Fig. 11. Robert O

Ritchie [35] concluded that for ductile (strain-controlled)

fracture, e.g., by micro-void coalescence (as in the present

case), the simple models suggest that the fracture

toughness KIc scales with the square root of the yield strength, multiplied by the elastic modulus, ductility and a

microstructural length-scale (e.g., which is some multiple of

the particle spacing). Fig. 20 shows failure mode in some

tested specimen as most nearly of them have the same model

and followed the same fracture mechanism, there is fibre

bridging and the crack path moves straight in some specimens

as in Fig. (20-C) the crack path steps and deviates through the

specimen. There are some surfaces damage and matrix

breakage and failure.



Table IV

Fracture surface release energy with different treatment

Specimens with treatments Average surface release energy GIC, (kJ/m2) S. D

(HCl 10% 1hr) 5.932 1.445083

(HCl 10% 2hr) 4.8626 0.861624

(HCl 20% 1hr) 4.5416 0.918844

(HCl 20% 2hr) 5.1674 1.343765

(HCl 50% 1hr) 5.6714 1.667443

(HCl 50% 2hr) 10.6658 2.25192

(Acetic acid 10% 1hr) 17.2826 2.857503

(Acetic acid 10% 2hr) 2.605 0.323548

(Acetic acid 20% 1hr) 4.8322 0.237906

(Acetic acid 20% 2hr) 9.5738 1.970719

(Acetic acid 50% 1hr) 4.0124 0.960957

(Acetic acid 50% 2hr) 4.764 0.199606

(Na OH 10% 1hr) 11.5124 1.798792

(Na OH 10% 2hr) 5.3138 0.224772

(Na OH 20% 1hr) 10.3546 1.045489

(Na OH 20% 2hr) 7.5614 1.41734

(Na OH 50%1 hr) 8.1622 0.951245

(Na OH 50%2 hr) 8.4714 0.5877

Fig. 16. load-displacement relation in compact tension test for HCl treatment a) 10 %, b) 20 %, c) 50 %

Fig. 17. load-displacement relation in compact tension test for NaOH treatment a) 10 %, b) 20 %, c) 50 %



8

Fig. 18. load-displacement relation in compact tension test for CH3COOH treatment a) 10 %, b) 20 %, c) 50 %

Fig. 19. Surface release energy variation with chemical treatment concentration at a) 1hr, b) 2hr boiling temperature

Fig. 20 Photograph of some failure sample of compact tension test

4. Conclusion

Date palm tree fibres (DPTF) are used as a natural

reinforcement to be an attractive agent in the composite

material industry. The chemical treatments program which

was introduced in the present paper gives a good enhancement

for the date palm tree fibres reinforced epoxy which

enhancement their debondablty with the epoxy resin. The

tensile properties of a composite reinforced by DPTFs which

has been treated by HCL chemically give better results and are

more compatible adhesive with the polymer matrix in all

concentration and time period, although they give quite little strength, while in other NaOH and CH3COOH the fibre

fractured, therefore, the strength sharply decreases. The same

results are concluded for fracture toughness which gives their

relationship with the composite tensile strength.

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