A REVIEW ON VARIOUS TECHNIQUES USED FOR...

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International Journal of Mechanical Engineering and Technology (IJMET) Volume 8, Issue 7, July 2017, pp. 1383–1395, Article ID: IJMET_08_07_150

Available online at http://www.iaeme.com/IJMET/issues.asp?JType=IJMET&VType=8&IType=7

ISSN Print: 0976-6340 and ISSN Online: 0976-6359

© IAEME Publication Scopus Indexed

A REVIEW ON VARIOUS TECHNIQUES USED

FOR SELF-HEALING IN FIBER REINFORCED

POLYMER COMPOSITES

Saurabh Saini

Assistant Professor, Mechanical Engineering,

Lovely Professional University, India.

Sandeep Kumar



Sandeep Pandey



Mohd. Zeeshan



ABSTRACT

The phenomenon of self-healing in polymeric composites has been inspired by

natural mechanism in which damage triggers the healing process. There has been a

huge interest over the past few decades in self-healing materials. Self-healing property

can improve material quality, lifetime and reduce repair costs. The system of self-

healing can be prepared from different types of polymers, chemicals and metallic

materials. This paper classify and characterize the various self-healing approaches,

methods, technologies and mechanism developed for fiber-reinforced polymer

composite (thermosetting) materials. Most of the approaches are inspired by natural

phenomenon of self-healing. Recent development in self-healing work has tried to

copy the natural process of self-repairing by vast and detailed study of the processes.

This approach for future developments in the field of self-healing is called bio-mimetic

approach. The aim is to initiate the work and develop the importance of various

approaches in the field of self-healing.

Key words: Self-healing, Polymer, Fiber reinforced, Bio-inspired, Thermosetting,

Composites.

A Review on Various Techniques Used for Self-Healing in Fiber Reinforced Polymer Composites


Cite this Article: Saurabh Saini , Sandeep Kumar, Sandeep Pandey, and Mohd.

Zeeshan A Review on Various Techniques Used for Self-Healing in Fiber Reinforced

Polymer Composites. International Journal of Mechanical Engineering and

Technology, 8(7), 2017, pp. 1383–1395.

http://www.iaeme.com/IJMET/issues.asp?JType=IJMET&VType=8&IType=7

1. INTRODUCTION

There is always a need and requirement in the development of material performance and

behaviour. Material development includes its design, analysis, quality, testing, performance

and maintenance. Development improves the performance of the material which is an

important aspect in determining the quality and cost effectiveness of any systems. Polymers

and composites are used widely these days. The damage in these materials is mainly due to

mechanical loading, chemical attack, thermal effect or a combination of several factors1.

Whenever there is damage in composite materials, their functional lifetime can be extended

by few available ways. Repair methods that can be applied directly on damaged area are ideal

repair methods. These ideal self-repair methods eliminate the need to change the component

for repair. Repair approach that work effectively for one damage mode might be not effective

for another damage mode. Therefore, the mode of damage plays an important part and hence

must be taken into consideration.

Hot plate welding was one of the earlier method for healing where polymer pieces above

the melting temperature of the material were brought into contact, and this contact was

maintained for long time at the crack face for interdiffusions to restore its strength. It has been

proved that the weld portion always remains the weakest point2. Resin is injected inside the

matrix to repair the damage in laminate composites. If the crack is beyond the reach of the

injection then this method fails. When there is a fibre breakage in composite laminates, a

patch is used to reinforce and restore the strength. Sometimes the resin injection along with

patch (reinforcing) is used to restore higher strength3. Both the repair methods are not ideal to

heal the material, as it requires a continuous monitoring and manual intervention. This

increases the cost of the material to a large extent.

This increases the interest in alternative approaches to heal the material. As the use of

composites is increasing day by day in automobile, construction, space and defence industries,

various techniques have been developed to repair the damage in the material. These

traditional methods of self-healing are not effective in case of micro cracks. In 1980s, first

self-healing concept in polymeric composites was proposed4. The aim of this approach is to

heal the invisible micro crack for increasing the service life of the material. Dry5 et al. in

1993 and then White6 et al. in 2001 took the attention of whole world and inspired them to

work in the area of self-healing in polymeric composites7. US defence organization8 Space

Agency (Europe)9 demonstrated the investments and huge amount of interest in self-healing

polymers. Due to high costs of active monitoring, self-healing materials can replace this

traditional method and expected to enhance the quality and service life of polymeric

composites. Throughout the development process of these smart materials, the source of

inspiration has been mimicking of biological systems (most of the biological systems are self-

healing in nature)10.

The main concern of this article is to consider the present work of self-healing in polymer

composites and to categorise the different healing approaches followed in the literature.

Purely review is not the only intension of this article, but to use and focus on bio-mimetic

approach that could advance the field further. There are many independent and complex self-

healing processes in nature that are worthy of study.

Saurabh Saini , Sandeep Kumar, Sandeep Pandey, and Mohd. Zeeshan


2. METHODOLOGY

Different self-healing approaches

2.1. Bio inspired Approach

New ideas for self-healing in engineering materials are inspired by natural technique of

damage repairing. Researchers, scientists and chemists have proposed various self-healing

concepts to restore the original strength after damage. Cross-link chains of polymer composite

can be broken due to damage and its strength can be restored by heat. Healing efficiency of

57% have been achieved11. In next example, solid-state polymer under the action of heat

migrates to the damage site12,13. This repairable solid-state polymer is the combination13 of

healing agent (thermoplastic) and thermosetting epoxy. These self-healing systems require

damage sensing mechanism that can trigger the heating requirement as soon as there is

damage. 14Later, the use of nanoparticles have considered as healing agent. These nanoparticles

were dispersed in polymeric layers to migrate at a damage site same like in blood clotting. An

integrated computer simulation is used for the study of nanoparticles within a multilayer

composite. Analysis of this model suggesting the possibility of a new self-healing mechanism.

The nanoparticles gradually migrate at the site of damage. The numerical models were

generated to estimate the load transfer to the nanoparticles from the matrix. This mechanism

is used in display technologies, communications and medical engineering. The mechanical

strength using nanoparticles can be restored upto 75%–100%. Later work15, has shown that

nanoparticles migrates and heals the crack in a thin layer of composite using its ligands. There

was no report for the restoration of mechanical strength.

The next study uses biological healing approach. In microencapsulation approach6,16,17

which involves the use of microcapsules (urea-formaldehyde) filled with dicyclopentadiene

(DCPD) were dispersed randomly within a polymer. When the microcapsule ruptures due to a

propagating crack, the healing agent is drawn along the crack where it meets a Grubbs

catalyst (Ruthenium based), initiating healing process. Polymerization of monomer and

catalyst was clearly seen to restore its strength that was lost from micro cracking within a

polymer matrix. Microcapsules can be placed with ease within a polymer matrix, which is the

main advantage of this approach. The need for fracture to release healing agent and the need

for the healing agent to encounter the catalyst to initiate healing process are the main

disadvantages of this approach. The size of microcapsules (typically 10-100μm) disturbs the

microstructure of matrix that causes additional problems. Due to clumping of microcapsules,

some results16,18 have shown decrease in healing efficiency.

Self-healing using hollow fibres is similar to the natural system using arteries. This

method is used in bulk concrete19,20,21,22,23 bulk polymers24 and polymers having millimetre

length scale25 and polymers having micrometre length scale26,27,28. Bleay26 used hollow glass

fibres that were filled with healing agent and embedded in a composite laminate. These

hollow fibres were used to make manufacture composite laminates. These hollow fibres are

used for self-healing and act as the reinforcement fibres. Poisson ratio effects can be reduced

by matching the orientation of hollow fibres and the fibres used for reinforcing the matrix.

The fibres location can be random to counter any failure threat. We can use different healing

resin based on requirement, different healing mechanism and mainly a significant volume of

resin can be made available. The need for fibre fracture and the low viscosity of healing agent

due to large diameter are the main drawbacks of hollow fibre healing system.

The ability to ‘see’ and taking precautions against any damage inside the material is

similar to the human body. Pang and Bond27,28 reported the mechanism in which there is a

formation of ‘bruise’ inside the composite material. In this work, they used a fluorescent dye



to design a damage visual enhancement method. This approach helps to identify the regions

for non-destructive evaluation. They also studied the rate of degradation of resin over the time

and infusion of dye into different damage sites with a C-scan (ultrasonic) NDE technique.

2.2. Bio-mimetic Approach

The study of biological system, processes and mechanisms to deliver the biomimetic healing

system has started in 200629,30. The development of engineering self-healing to biomimetic

process is a challenge for future. This approach is still in its early stage but the natural

phenomenon of bruising, clotting and healing network has been considered. Self-healing

material in engineering materials are either randomly distributed or evenly spaced. Natural

self-healing mechanism has network that is made for a specific function. First case of

detecting the site of damage and healing in polymeric composite is reported by Trask31,32. The

main failure points were identified and then setup using hollow fibers for self-healing was

designed for a particular composite material. The importance and need for self-healing

increases the demand of the healing agent specifically in terms of mechanical strength. This

setup was found to restore significant mechanical strength.

Figure 1 Vascular network self-healing. Adapted from53

Table 1 provides the summary of the biological healing methods and compare them

against the process/mechanism currently used in research for engineering materials



Table 1 Summary of healing approaches followed

3. EXPERIMENTAL RESULTS

3.1. Mechanical tests for computing healing efficiency

Healing of polymer composite refers to the restoration of various mechanical strength. It is

not possible to measure the extent of healing because various properties are healed and

restored. Wool33 et al. suggested a method to define the healing efficiency in composite

material. This approach has been adopted and used to find the “healing efficiency” of

composites. For every mode of failure, there is a unique method to find its respective healing

efficiency. This is the reason that makes quantifying the limit of healing in composite

material.

3.2. Fracture test

The susceptibility to fracture in a given material can be expressed as KIC (plane strain fracture

toughness).Healing ability of the material can be expressed by comparing the fracture

toughness. The healing efficiency is η,

Biological mechanism Polymer/Chemical or

Engineering material

Self-healing approach

used in application

References

Self-healing concept Polymers/composites Bioinspired self-healing

approach that require external

source to initiate repair.

[11]

Capsules Bleeding action in which

healing agent is stored in a

container embedded within the

matrix.

[16,17]

Bleeding Hollow fibres Bleeding action in which

healing agent is stored in

reinforcement material and

activates after the damage

initiation within structure.

[26]

Blood cells Nano-particles Artificial cells that have the

capability of depositing nano-

particles at the damage site.

[14]

Vascular network Hollow fibres A network that maintain the

continuous supply and flow of

healing agent throughout the

structure.

[53]

Blood clotting Resin Specially designed resin to

heal the damaged site locally. [31]

Bone repairing Reinforcing fibres Deposition, absorption, and

rebuilding of damaged

reinforcing fibres.

[31]



Ƞ�%� ��

��

�100

In taper double cantilever beam (TDCB) test, evaluation of healing efficiency begins with

a virgin fracture test. A precrack is introduced in the specimen and the load is gradually

increased until the final failure due to the propagating crack throughout the sample. At room

temperature, the sample is then allowed to heal without any external disturbance. After

complete healing of the specimen, it is loaded until complete failure. Newly developed and

verified TDCB geometry is given figure 2.

Figure 2 ASTM of Taper double-cantilever beam test (dimensions in mm)

3.2 Tensile test

In tensile testing, healing of interfacial de-bonding and fiber-reinforced epoxy composite was

investigated. In sample preparation, an epoxy mixture with DCPD 30wt% and Grubb’s

catalyst 2.5wt% was prepared. Strands of fiber were coated with this epoxy mixture. These

fibers were then embedded in the matrix resin. After a healing time of 48 hours, 14% healing

efficiency was achieved at room temperature.

3.3 Fatigue Test

Fatigue test is performed to examine the material behaviour and its healing efficiency for

dynamic loading. It is no longer meaningful to compute healing efficiency at static loading. A

new term ‘life extension factor’ was introduced to define healing efficiency34. An

investigation on the behaviour of the healing epoxy at the time of fatigue crack propagation

was according to rules and constraints.



Ƞ�%� �� !"��

�

Where ��and �� !"��are defined as the number of cycles required for failure for a

self-healing and without healing sample respectively. Fatigue depends on factors like healing

kinetics, stress range, ratio of stress intensity, loading frequency and the rest periods

employed35. This is the reason that makes the evaluation of healing efficiency for fatigue

loading more complex.

3.4. Tear test

Healing efficiency for a tear specimen is defined as the recovery of tear strength, where

Ƞ# � T%&'(&) � T*+,-+.

In tear test, the specimen is made from a rectangular strip. This strip has two loading arms

which were formed due to a significant axial precut that. The specimen is loaded until the tear

propagates through the specimen shown in Figure 3.Evaluation of healing efficiency starts

with a tear test for virgin sample. The sample was kept at room temperature for healing after

failure without any external disturbance. After healing time, the tear sample is loaded again

until failure. It was reported that above 70% of tear strength was recovered in the

(polydimethylsiloxane) system36.

Figure 3 Tear test setup

3.5. Flexural test

In this test, the mode of failure is bending. The test setup consists of an indenter, which is

used to apply the point load at the center of the sample. The rollers at the two extreme ends

support the sample. The setup is shown in figure 4 below. The maximum healing efficiency

achieved in this test is 93%. Virgin sample is first loaded until the complete fracture of the

sample. Later, the specimen having healing capability is loaded until the fracture and then left

for 48 hours to self heal the damage sites. Then finally, the healed sample is evaluated until

the complete failure. These steps were followed to quantify the healing efficiency. Table 2

provides summary of all approaches, testing method used for self-healing in composites and

their respective healing efficiency evaluated.



Figure 4 Three-point loading of the specimen

Table 2 Summary of development achieved in self-healing of polymer composites.

Healing mechanism Physical

medium

Highest

efficiency

Environment

condition Type of loading Ref.

Thermosetting

Composites

Hollow glass fiber

Mechanical

93% 24 hours at

ambient atm. Flexure Strength [19–29]

Microencapsulation

Approach

80–93%

48 hours at

800C,24 hours

at room temp

and again 24

hours at 800C.

Tensile loading,

Fatigue

strength and

toughness

[16,17]

Micro-vascular

network

60–70%

7–30 cycles

12 hours at

ambient atm.

Fracture

toughness [53]

Thermoplastic

additives 30–100%

2 hours at

1500C, 10 min

at 1200C

Fracture

toughness,

Tensile and

Flexural loading.

[12,13]

Carbon fiber 46%

70–120◦C

for 10-20

minutes.

Impact strength [54]

Silicone

(elastomer) Rubber

65–95%

45-48 hours at

room condition.

Strength in tear

failure. [55]

Thermoplastic

Diffusion 100% 60◦C for 5

minutes. Impact loading [56]

Healing(light-

incident) 26%

1000C for 10

minutes. Flexural loading

3.6. Chemicals used for self-healing

Table 3 provides a summary of all the different types of chemicals used for self-healing. The

phenomenon of self-healing due to these chemicals is based on ring formation of monomer.

This process is called ring-opening metathesis polymerization (ROMP). This mechanism of

ring formation has inspired and attracted many scientists and researchers. Obviously, there are

some similarities between hollow fibres and microcapsulation approach, but compared to

hollow fibres, microcapsules eliminate the manufacturing process. This microencapsulation



technique is also used in brittle material such as glass and ceramics37. DCPD is the first

chemical, which is used as a healing agent. After many trials and experiments, 5-ethylidene-2-

norbornene (ENB)38 was suggested to replace DCPD as a healing liquid. Blending ENB with

DCPD39 was also tried to improve the healing efficiency. This ENB was also used in

microencapsulation self-healing approach. DCPD has low melting point and uses large

amount of catalyst. This limitation is supposed to overcome with the use of ENB. It is

reported that DCPD forms a ring structure (cross-linked) whereas ENB polymerizes to give

linear chain formation. This cross-linked structure possesses high strength compared to linear

chain structure40,41. However, ENB has high melting point, reacts faster and requires lower

amount of catalyst (Grubb’s)38. A mixture of DCPD and ENB was supposed to give an

enhanced result in terms of strength and reactivity time. Cho42 et al. developed a new healing

system in which healing agent is a mixture of HOPDMS (hydroxyl end-functionalized

polydimethyl-siloxane) and PDES (polydiethoxysiloxane) and using di-n-butyltin dilaurate

(DBTL) as the catalyst. The polymerization of healing agent and catalyst occurs rapidly and at

ambient room condition. This rapid reaction takes place in the presence of organotin43,44.

Table 3 Chemicals used in self-healing process

4. FUTURE SCOPE

Finally, we know that the material can fail with many reasons, such as thermal effects, fatigue

loadings, corrosion or environmental of all kinds. Material failure generally starts at the

micro-scale level. Later, it propagates to the higher level until failure occurs. The best solution

to avoid this sudden failure is to restrict damage at the micro scale level. This idea would help

to restore the original properties of material. In case of a bullet penetration, heat energy is

used to initiate the healing process46. To date, all the self-healing methods have the limitations

by the size of container. Large hollow cavities formed due to large container size could

change the microstructure of the material12. It would be ideal to have a material that could be

tougher and self-repairable at the same time. Carbon nanotubes (CNTs) can be used for

storage devices as well as mechanical reinforcement because of their high strength and small

size. They have the hollow tubular structure. Some materials such as hydrogen, C60, DNA,

metal carbide and CH447,48,49,50,51 have been inserted inside CNT. The use of CNTs as

container/reservoirs for healing agent has been considered for self-healing applications52.

Self-healing agent Catalyst Reaction References

Dicyclopentadiene

(DCPD)

Grubbs’ catalyst (ruthenium (IV)

based) ROMP [21, 22, ]

5-Ethylidene-2-

norbornene (ENB)

Grubbs’ catalyst (ruthenium (IV)

based) ROMP [38]

DCPD/ENB blends Grubbs’ catalyst (ruthenium (IV)

based) ROMP [39]

Mixture of hydroxyl end

functionalized

Polydimethyl siloxane

(HOPMDS) and

Polydiethoxysiloxane

(PDES)

Di-n-butyltin dilaurate Polycondensation [42]

Epoxy Amine Polycondensation [45]



Figure 5 demonstrates the use of CNTs to carry the healing agent and also as a filler material

after the delivery of healing agent for restoration of mechanical strength.

.

Crack Catalyst Matrix Released healing agent Healed crack

Figure 5 Self-healing using CNT. Adapted from52

5. CONCLUSION

Damage initiation at the nano-scale level, damage propagation and tolerance has limited the

use of composite materials. This phenomenon of self-healing in a damaged composite

material results in composites with increased service life. Over the last decade, new

technology and method of self-healing have been emerging because of financial constraints in

microencapsulation and hollow fibres. Self-healing approaches for composites have primarily

been bioinspired. Biomimetic self-healing approach is the most recent advance work. Detailed

study of vascular networks is the most recent, active and interesting research topic of self-

healing. To implement this vascular network (biomimetic approach), ideal healing agent is

required for this system. Reinforcement could increase the service life incase of matrix

dominated failure modes. Innovative concepts, interesting ideas and new technology has

opened the design of smart self-healing nanosystems. Computer generated numerical models

and simulations have provided relevant useful information to researchers and scientists

towards the design and fabrication of self-healing systems.

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