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Recent trends in Activated Carbon Fibers production from various

precursors and applications—A comparative review

Muhammad Faheem Hassan, Muhammad Ashraf Sabri, Hammad

Fazal, Ainee Hafeez, Nasir Shahzad, Murid Hussain

PII: S0165-2370(19)30322-5
DOI: https://doi.org/10.1016/j.jaap.2019.104715
Reference: JAAP 104715

To appear in: Journal of Analytical and Applied Pyrolysis

Received Date: 3 May 2019

Revised Date: 16 October 2019
Accepted Date: 17 October 2019

Please cite this article as: Hassan MF, Sabri MA, Fazal H, Hafeez A, Shahzad N, Hussain M,
Recent trends in Activated Carbon Fibers production from various precursors and
applications—A comparative review, Journal of Analytical and Applied Pyrolysis (2019),
doi: https://doi.org/10.1016/j.jaap.2019.104715

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© 2019 Published by Elsevier.

Recent trends in Activated Carbon Fibers production from various precursors and applications
– A comparative review

Muhammad Faheem Hassana, Muhammad Ashraf Sabrib, Hammad Fazalb, Ainee Hafeeza, Nasir
Shahzada, Murid Hussaina,*
aDepartment of Chemical Engineering, COMSATS University Islamabad, Lahore Campus,
Pakistan
bDepartment of Chemical Engineering, Muhammad Nawaz Sharif University of Engineering and
Technology, Multan Pakistan

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Graphical Abstract

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Highlights:

 Comparison between synthetic precursors and natural precursors for activated carbon
fiber (ACF).
 Practicality of lignocellulosic precursor based ACF to be used in industrial application

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  Advantages of lignocellulosic precursors as ecofriendly, economical, sustainable, and
renewability
 Practicality of lignocellulosic precursor based ACF for co-production of biochar and
bioenergy in combined pyrolysis-combustion process

Abstract:
Activated carbon fibers (ACF) are relatively novel and by far one of the most important fibrous

carbon materials owing to their special characteristics such as fibrous structure, high porosity,

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high volumetric capacity, excellent packing density, fast adsorption kinetics, good porous

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storage capacity and ease of handling. This work aims to present a detailed overview of

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activated carbon fiber (ACF) synthesis process, influence of the process variables on the

morphology of these ACF and their applications. A comprehensive study of major precursors
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(polyacrylonitrile, pitch, phenolic and cellulosic), particularly comparison between the

characteristics of ACF based on these precursors, has been provided with an eye for details.
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Among them, lignocellulosic based ACF are suitable solutions for industrial scale ACF production

implementing cost effective and environment friendly approach. The use of lignocellulosic
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material for ACF has the potential to reduce greenhouse gas effects and is a suitable alternative

for solid waste management of lignocellulosic solid produced annually. Furthermore, reports on
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the applications of ACF in CO2 capture, volatile organic removal, wastewater treatment and
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energy have also been critically reviewed. ACF currently hold small market component of

specific high-end uses. Due to their unique characteristics and advantages over other carbon

materials, ACF can be anticipated to dominate a major market in the emerging areas of smart

fabrics, energy storage, health care, water and air purification and advanced instrumentation.

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Keywords: Lignocellulose, adsorption, activation, pore size distribution, CO2 capture, Energy

1. Introduction

1.1 Activated Carbon Materials

Activated carbon materials (AC), traditionally termed as activated charcoal, are well-known

porous materials in carbon family characterized by their complex structure of carbon atoms [1,

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2]. AC are excellent adsorbents exhibiting immense adsorption capacities for adsorption from

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liquid and gas phases due to their high surface areas and tunable pore structures [3, 4]. Human

kind has been exploiting the versatile nature of AC from ancient Egyptian era (3750BC) by

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employing it and its derivatives like biochar and charcoal to enhance land fertility, as a fuel, and
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in medical applications, to name a few [5-7]. Though the industrial applications of AC were first

reported in late 1800s when AC were first used as adsorbent in water treatment [8] however
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the industrial manufacture and extensive modern research of AC can be dated back to early

1900s [5, 9]. Since then porous carbon materials, such as activated carbon (AC) and activated
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carbon fibers (ACF) and other forms of carbon materials, such as carbon fiber (CF) have become

the center of attraction for labs and industries all over the world. AC are manufactured either in
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powdered form with a particle size less than 100 µm and an average diameter of 100 µm or
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granular shapes with a particle size ranging from 100 µm to several millimeters depending upon

the industrial applications [10]. Almost all carbon-rich precursors including entire world’s flora

can be converted to AC through stabilization (if required), carbonization and activation [11, 12].

The details of stabilization, carbonization and activation are discussed in section 3. Several

factors such as cost, availability, ease in activation, renewability, inorganic content and carbon

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yield influence the choice of precursors used for AC production. Several low-cost precursors are

lignite, coconut, pistachio shell, saw dust, charcoal, peat, rice husk, bituminous and brown coal,

walnut, agricultural waste and petroleum coke [13-29]. AC in different particulate forms such as

granular active carbons (GAC), powdered activated carbons (PAC) and extruded active carbons

(EAC) have widespread use in broad spectrum of industrial applications including, but not

limited to, water and gas purification, liquid and gas effluent treatments, gas storage, catalysis,

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metal recovery and biomedical applications [5, 20, 30-37]. The difficultly in handling of these

particulate forms of AC in industrial applications are a reason, among few others, for relatively

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limited end-use applications of AC despite its remarkable properties [5]. As a result of pursuit of

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a unique material that could alone fit the vast majority of industrial requirements [5-8, 38],

such as high tensile strength, low weight and high temperature tolerance, CF and ACF were
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manufactured from cellulosic fibers, synthetic and natural materials in 1960s [39-41].
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1.2 Carbon Fibers

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Carbon fibers (CF) are the carbonaceous materials having a fibrous shape and a diameter of 5-

10 µm [42]. The International Union of Pure and Applied Chemistry (IUPAC) has defined CF as
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filaments, lines, fibers or reals containing at least 92 wt.% carbon, usually in a nongraphitic

state [11, 42]. The nongraphitic state is characterized as a long-range two-dimensional order of
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carbon atoms in planar hexagonal networks without any crystallographic order in the third

direction aside from more or less parallel stacking [11, 43].

Carbon fibers (CF) inherently have excellent tensile strength, phenomenally low weight, low

thermal conductivity, high chemical resistance and better temperature tolerance. These

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qualities make CF a highly sought-after choice in aeronautics, automobile, sports, civil

engineering and other such applications [11, 44-47].

The production of CF from organic precursors, such as Polyacrylonitrile (PAN), involves spinning

(melt spinning, dry spinning, wet spinning) of organic precursors into fibrous form, thermal

stabilization in air to render the precursor infusible and carbonization at elevated temperatures

in an inert atmosphere (usually nitrogen) [11, 48, 49]. In general, CF can be considered as the

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prognosticator of ACF as latter shares same basic manufacturing steps as CF [11]. Although

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most industrial applications were met by AC and CF materials combined, the search for a

material that could alone fit the requirements of vast majority of industrial applications

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continued. As a result, ACF were first produced in 1960s for resistant textile bearing a
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resemblance to CF (fibrous) and have structure similarity with AC materials (highly porosity)

[49].
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1.3 Activated Carbon Fibers

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Activated carbon fibers (ACF) are highly porous materials in fibrous form having an aspect ratio

of at least 10, a well-define porous structure and narrow pore size distribution [42, 50]. Though
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ACF show similar properties, such as porosity, to AC [51] yet offer several other advantages
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owing to its fibrous shape. ACF is an excellent microporous material with negligible

mesoporosity and negligible to none macroporosity [52]. The classification of ACF,

recommended by International Union of Pure and Applied Chemistry (IUPAC), is demonstrated

in Figure 1. [11, 52]. Ting Lee mentions ACF as a hybrid of AC and CF [11]. Though ingenious yet

care should be taken while addressing ACF as a hybrid. The ACF is, essentially, the intersection

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of activated carbons and carbon fibers. The carbon fibers are activated to produce activated

carbon fibers; thus it is not a composite material as the word “hybrid” might suggest [53].

Remarkable characteristics of ACF like excellent volumetric capacity, high packing density, high

specific surface area with uniform micropore volume, outstanding adsorption capacity, fast

sorption/desorption rates, enhanced design flexibility and ease of regeneration affirm its

efficacy in adsorption applications [5, 11, 42, 51, 54-57]. Over the past few decades, ACF has

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overruled several contemporary competing materials, having intersecting applications with ACF

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such as activated alumina, AC, CF and zeolites, because of its unique and well-developed

structural properties [58-62]. ACF has attracted significant attention in recent years due to

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these characteristics and potential applications in a large number of small- and large-scale
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industrial applications. Its improved and tunable micro and meso porosity enables it to have

applications in predominant-research fields i.e. natural gas storage, adsorbent in heavy metal
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industry, treatment and purification of water and air, hydrogen storage as a fuel, and

electrochemical applications such as supercapacitors [11, 54, 61, 63, 64]. Meanwhile its vast
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applications in textile industry include personal protective clothing, domestic fabrics, medical

masks, filtration, and catalytic support [65-69].

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Several book chapters, research papers and reviews have been dedicated to the discussion of
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ACF [10, 11, 70-74]. A current literature search shows that around 4500 articles (including book

chapters, research papers and reviews) have been published relating to ACF. Figure 2

demonstrations that the number of publications on ACF, as of 1995 – 2019, kept on increasing

with highest number of publications in 2017-2019. The most recent comprehensive review by

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Ting Lee et al. summarizes the production of ACF providing comparisons of various precursors,

applications of ACF for end-use [11]. Much has improved since then related to the

understanding of ACF, availability of renewable precursors and potential applications of ACF

keeping in view the carbon footprints and environmental obligations. Thus, currently there

exists a need for a review article comparing the present precursors particularly of renewable

bio-origin such as biowaste and agricultural wastes, end-use applications and assimilation of

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un-coordinated information into a comprehensive text. This manuscript is an effort for such a

comprehensive review.

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2. Activated Carbons, Carbon Fibers and Activated Carbon Fibers

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ACF are a hybrid of AC and CF. The advantages of ACF over other forms of ACs are its high
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porosity and higher adsorption rates. However, the cost and extra processing step of converting
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the initial material into fibrous form is a major disadvantage of ACF. The characteristics,

advantages and disadvantages of AC and ACF have been presented in detail in Table 1. It is
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interesting to note that the ACF are quite different from CF even though both share the similar

thermochemical process for their production. CF feature exceptional tensile strength (3000 –
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7000 MPa) in comparison to ACF with low tensile strength (70 – 400 MPa). In contrast, ACF

provides extraordinary porous structure and high specific surface area (> 3000 m2/g). Such high
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specific surface area and high micropore volume features high adsorption kinetics and

capacities of ACF. A detailed study on the differences between the characteristics of CF and ACF

has been provided by Chen [5].

3. ACF Processing Steps

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Processing of ACF from precursors, such as phenolic resin, polyacrylonitrile (PAN), viscous ryan,

pitch, polyamide fiber, asphalt fibers, saran, polymeric fibrous materials, lignin and renewable

biomass (with high lignocellulosic, hemocellulosic and lignin contents), involves the same steps

as conducted in the preparation of traditional carbon fiber except for an additional step of

activation of CF, where pore distribution of the precursor is further developed and matured [11,

74, 75]. The steps involved in ACF production are spinning, stabilization, pre-treatment e.g. acid

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impregnation (prior to carbonization), carbonization/pyrolysis and activation. It should be

noted though, that the spinning, pretreatment and stabilization steps are precursor-dependent

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and are not always included in the ACF production. Generally, ACF can be synthesized through

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carbonization and activation (either chemical or physical) processes. The generalized flow

diagram of ACF processing and production from various precursors and ACF end-uses in
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wastewater treatment, VOC removal, energy and carbon dioxide capture has been illustrated in
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Figure 3.

3.1 Spinning
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Spinning process induces fiber form in organic precursors, such as PAN. Different spinning
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techniques i.e. dry spinning, melt spinning and wet spinning are employed depending upon the

nature of the precursor [5, 11, 48, 49]. Spinning temperature is usually set slightly higher than
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the softening point of the pitch [76]. In melt spinning, disordered planar aromatic viscous

thermoplastic materials like pitches and resins are turned into fibers by changing the

orientations of the molecules from random to along the axis of the fibers [77, 78]. The fibrous

precursors are, then, subsequently converted to CF through carbonization and subjected to

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activation thus converting the CF into ACF. A detailed discussion on carbon fiber spinning can

be found elsewhere [79].

3.2 Stabilization

Oxidative stabilization of the spun (to filaments) precursors involves thermal treatment(s) at

different temperature ranges depending upon the precursors but usually the temperature is set

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in the range of 423 – 673 K or above usually in the presence of oxygen [57, 80, 81]. Cross linking

of the aromatic molecules occurs during oxidation inducing non-diffusivity, heat resistivity and

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preserve the fibers by converting thermoplastic fibers (pitches and resins) into thermosetting

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and formation of ring chain in PAN molecules [82-85]. The degree of stabilization, if required as

in PAN fibers, is an important factor in ACF production as it defines the mechanical and thermal
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properties of the oxidized fibers that consequently determines the properties of final product
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(ACF) [83, 86]

3.3 Carbonization
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High temperature treatment of carbonaceous substrate in the absence of air and in the
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presence of inert medium (N2, argon) that removes the volatile organics either in the form of

gases such as CO2, CO, H2O or condensed liquids is known as carbonization [57]. The resulting
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product is char which contain pure carbon structure with small amount of nitrogen and

hydrogen. In simpler words, carbonization of organic material results in a solid residue with

increasing content of carbon (element) by pyrolysis in an inert environment [43]. Temperature

of the carbonization depends on the applications of the char produced in carbonization, and for

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ACF production is usually done at temperature below 1573 K [57, 80]. Carbonization involves

several complex physiochemical changes like dehydrogenative condensation (loss of H2

followed by the formation of larger planar molecular network), polymerization, aromatization

and removal of almost every single inorganic impurity like oxygen, nitrogen, carbon monoxide,

methane, hydrogen, and water from the fiber resulting in over 90% carbon fiber [80, 87].

Generally, carbonization induces high thermal and chemical resistance, better conductivity and

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dimensional stability [57]

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Depending on the nature of the precursors, pretreatments such as pre-oxidation or

impregnation with chemicals is required before carbonization to enhance the yield, strength

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and adsorption capacities of the final product [56]. However, the inclusion of an extra step
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(pretreatment) increases processing and production costs. Thus, direct carbonization step is

preferred, if possible, to save time and energy. To achieve maximum yield of char, careful
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examination of pyrolysis conditions is required since minor variations in retention time or

temperature can lead to drastic changes in the yield of final product [57].
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3.4 Activation (Physical vs Chemical)

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Vigorous heat treatment in the carbonization process leaves some pores blocked with
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disorganized carbon. Activation process removes the disorganized carbon, enhances the pore

distribution and can also enlarge the already developed pores. Two kinds of activation

processes viz. physical and chemical activation have been reported in the literature [57, 88-90].

In physical activation process, char is heated at temperature between 973 to 1473 K in an

oxidizing environment like CO2, steam, or combination of steam and N2 [57, 91-95].

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Steam usually produces wide pore size distribution with pores ranging in mesoporous region

while CO2 produces pores in microporous region and hence higher overall pore volume [96, 97].

Zhang et al. reported the production of polyvinyl-alcohol (PVA) based ACF (PVA-ACF) under

carbon dioxide, air and steam activations. Under identical activation conditions, the carbon

dioxide activated PVA-ACF had the highest pore volume and surface area in comparison to pore

volume and surface area of air and steam activated samples [95].

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In chemical activation, char or CF are typically heated at a temperature range of 673 to 973 K in

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an inert atmosphere along with a chemical agent. Acids like phosphoric, sulfuric or hydroxide

such as sodium, potassium or a chloride of hydrogen or zinc could be used as a chemical agent

in chemical activation process [57, 90, 91, 98, 99].

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Both types of activation process involve their own typical pros and cons. Low overall cost of the
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process is only but main advantage of physical activation over chemical activation [100]. On the

other end, chemical activation advantages include better micropore distribution at low
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temperature range in least time frame [51, 101-104]. In activation processes, heating trends

have changed from conventional thermal methods – that consumes more energy and time with
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low output – to latest microwave assisted technique which in turn is, specific, faster,

homogenous and a more efficient way of heating [56, 105-108].

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4. Precursors for ACF Production

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There are four major precursors for the production of ACF namely polyacrylonitrile (PAN),

phenolic resins, pitch resins and bio-based materials like lignocellulosic material. The details of

these have been presented in the preceding paragraphs.

4.1 Polyacrylonitrile (PAN)-based ACF

PAN, also known as polyacrylonitrile, is a synthetic thermoplastic polymer with the chemical

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formula of (C3H3N)n. It is a semi-crystalline polymer with melting and glass transition

temperature of 623 K and 353 K, respectively [57, 109]. Production of activated carbon fibers

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from PAN-based fibers is usually a three-step process namely thermo-oxidative stabilization,

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carbonization and activation under certain environment and controlled conditions [57, 80]. The

formation process of PAN based activated carbon fibers is shown in the Figure 4. Thermo-
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oxidative stabilization of PAN fibers is mostly carried out under oxygen environment, such as
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air, at a temperature range of 473 K – 623 K [57, 80]. Mathur et al. reported that thermo-

oxidative stabilization of PAN fibers below 573 K results in an incomplete stabilization of the
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precursor resulting in poor properties after carbonization [110]. A temperature range of 623 K –

673 K is suggested for suitable stabilization of PAN fibers to ensure enhanced carbon fiber
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characteristics [110]. Similar approach has been reported by other researchers [111, 112].
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The stabilization of PAN fibers converts it from thermally unstable thermoplastic polymer to

thermally stable thermosetting solid ready to be carbonized at elevated temperatures. The

stabilization of PAN fibers is a time-consuming task and involves various reactions such as

cyclization, dehydration and oxidation. The primary stabilization mechanism, the related

reactions and change in morphology of the PAN fibers, because of these changes, have been

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discussed in detail by various researchers [57, 80, 112, 113]. Nevertheless, it is worth

mentioning that the thermal stability and infusibility of stabilized PAN fibers at elevated

temperatures are a result of stable ladder polymeric structure and cross-linkage between PAN

molecules formed during stabilization [57, 114].

Stabilization precedes carbonization, or pyrolysis, of PAN fibers normally at a much lower

temperature than the latter. Carbonization for PAN fibers is done at elevated temperatures

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ranging from 973 K to 1373 K. However, the production of high performance carbon fibers

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requires elevated temperatures up to 1573 K. Frank et al. summarized the chemistry,

performance, structural features and the influence of the production processes such as

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stabilization, pyrolysis, activation and surface treatment on these characteristics [115]. The
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pyrolysis of PAN fibers removes typically all the non-carbon elements leaving fibers high in

carbon percentage (>92 percent). Dehydration, dehydrogenation, intermolecular cross-linkage,

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coalesce of cyclized sections by cross-linkage, denitrogenation and evolution of gases results in

the formation of disordered graphite-like structure of the carbonized fibers [80, 113, 116]. The
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mechanism, structural changes and chemical transformations of PAN fibers during

carbonization have been investigated in relation to carbonization temperature and physical

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characteristics of PAN fibers [57, 80, 113, 116, 117]. Frank et al. in his review, reported model
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reactions pathways of stabilization and carbonization of PAN fibers [82]. Pyrolysis of PAN fibers

releases significant amounts of various volatile products such as water, hydrogen, and nitrogen

including hazardous gases such as hydrogen cyanide, carbon monoxide, carbon dioxide,

methane and ammonia [57]. Thus, special precautions must be taken to handle these released

gases during pyrolysis.

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Activation of carbonized fiber is the final step in achieving the ACF from PAN fibers. Activation is

typically carried out under an inert atmosphere, mostly nitrogen flow at a temperature of 573 –

1173 K and 773 – 1473 K for chemical and physical activation, respectively. The selection of

optimum temperature, residence time, heating rate, the flowrate of gases (oxygen or air for

stabilization and inert for carbonization or activation) and the type of activation agent for PAN-

based ACF depends primarily on the precursor, width of the fibers and the required final

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properties. The final structure and morphology of the ACF depends mainly on the precursor and

process conditions of stabilization, carbonization and activation [118, 119].

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Amaral Junior et al. reported the production of microporous ACF from textile PAN fiber with a

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surface area of 1260 m2/g using CO2 activation at a temperature of 1173 K [94]. PAN fiber based
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ACF were prepared by steam activation (923 – 1273 K) and KOH activation (873 – 1073 K). The

results demonstrated that the surface area for KOH activated ACF is significantly higher than
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steam activated ACF [119]. The higher temperature and impregnation ratios increase the

surface area of ACF to a maximum value. Further increment in activation temperature or

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impregnation ratio destroys the fibrous morphology of the ACF resulting in a smaller surface

area [119, 120]. Doaa et al. successfully prepared PAN fiber based ACF by stabilization and
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carbonization at 523 and 1123 K, respectively with the heating rate of 10 K/min. The KOH
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activated ACF possessed a specific surface area of 2800 m2/g at an impregnation ratio of 3:1.

The resultant fibers were reported to retain the fibrous structure. On the other hand, steam

activated ACF possessed a maximum surface area of merely 774 m2/g [49]. One of the major

disadvantages of PAN fiber based ACF, apart from its high cost, is the use of toxic chemicals for

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its preparation. Such practice in industrial application is not suitable in terms of safety

regulations, sustainability and environment friendly practices.

ACF can be produced from single precursor or a combination of precursors to enhance the

targeted property of the finalized product. For example, PAN fibers are known for their

excellent fiber-formation characteristics while pitch offers higher conductivity and surface area

[119, 121]. Bui et al. derived ACF from PAN/pitch based electro-spun fibers to utilize the

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combined advantages of both precursors. ACF were derived using steam activation at different

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temperatures (973 – 1173 K). The specific surface area of these ACF ranged from 732 – 1877

m2/g as the activation temperature increased from 973 – 1173 K. Increasing the temperature

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results in increased surface area of the ACF up to a maximum value. Further increase in the
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activation temperature, decreases the surface area as a result of burn-out and destruction of

microscopic pores [121].

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It has been established that PAN-based carbon fiber is stronger than other type of precursor-
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based carbon fiber [6]. PAN-based fibers have been found to be the most suitable precursors

for producing high performance carbon fibers (compared to pitch, rayon, etc.) generally
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because of its higher melting point, greater carbon yield (>50% of the original precursor mass)

and fast pyrolysis rate [7, 8, 38, 39]. Although carbon fiber can be derived from pitch precursor,
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processing and purifying it to the fiber form is very expensive as compared to PAN-based fibers

[41]. PAN with molecular formula [C3H3N]n can produce carbon fiber of relatively high carbon

yield giving rise to a thermally stable, extremely oriented molecular structure when subjected

to a low temperature treatment [11]. PAN fiber was also preferred to be the precursor because

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of its fast rate in pyrolysis without changing its basic structure [11]. Optimizing the pyrolysis of

PAN precursor fiber would ideally result in enhanced performance of the resulting CF that can

then be converted into high performance ACF. Few examples of synthesis parameters, pore size

distributions, total surface area and applications of PAN-based ACF are given in Table 2.

4.2 Pitch-based ACF

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Pitch, in general, is a viscid complex mixture of aromatic hydrocarbons and heterocyclic

compounds obtained as a residue from heat treatment or distillation of petroleum fractions or

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coal tar [43, 57, 85]. Marsh et al. mentioned pitch to be a residue from tar distillation or

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pyrolysis of organic material [43]. Variations in pitches composition and average molecular

weights depending on their origin and processing methods [85, 123, 124]. The average
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molecular weight of pitches is around 200 – 400, however the molecular weight of constituents
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can range from 200 to 2000 g/mol [85, 124, 125]. Pitches have been reported to exhibit broad

softening temperature ranges instead of a single melting point [43, 85].

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Isotropic pitches can be converted to mesophase pitches upon thermal treatments at 623 – 723

K [85, 123]. Heat treatments facilitate polymerization and aromatization reactions within the
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molecules of the pitch thus converting isotropic pitch into mesophase pitch [85, 123]. Detailed
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discussion on the mesophase and isotropic pitch is found elsewhere [85, 123].

Spun pitch fibers need stabilization with O2 to render these fibers infusible for high

temperature treatments during carbonization [126, 127]. Oxidative stabilization of pitch fibers

is usually done in a temperature range of 423 to 573 K [57, 128, 129]. An oxygen content of 10

16
to 23% is proposed to be best for oxidative stabilization [57]. This oxidative stabilization uphold

the axial directed aromatic molecules and induce cross-linking among molecules within the

fibers turning thermoplastic fibers into thermosetting [130].

Pitch-based CF can be categorized into general performance CF (GPCF) and high performance

CF (HPCF) [123]. Isotropic pitch is mainly used for the production of the former while

anisotropic or mesophase pitch is used for the production of the latter [123]. Conventional

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usage of GPCF is in application such as thermal insulations, reinforced concrete or electrode

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material and for manufacturing activated carbon fibers e.g. for adsorption, water purification

[123, 131, 132]. In principle, the mesophase pitch can be converted to activated carbon fiber

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through the steps mentioned in section 3. However, the use of expensive mesophase pitch for
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GPCF application, such as ACF production, is cost-prohibitive and should be avoided. Under

similar activation parameters, mesophase pitch-based CF are reported to have higher oxidation
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resistance to CO2 during heat treatment of CF and result in much lesser surface area as

compared to isotropic pitch-based CF [57, 133]. Hence, as a precursor for carbon materials for
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GPCF applications, isotropic pitches instead of mesophase pitches should be used to produce

AC, carbon membranes, CF, and ACF. The usage, preparation and details of mesophase pitch
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based CF as HPCF can be found elsewhere and is out of the scope of this article [123]. Detail of
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ACF from PP and CTP are given below:

4.2.1 Coal tar pitch (CTP) based ACF

Coal tar pitch (CTP), residue of heat treatment or distillation of coal tar, is quite abundant and is

a common name for complex mixture of thousands of hydrocarbons mainly aromatic

17
hydrocarbons and heterocyclic compounds [43, 85, 134]. CTP often have low softening point

(SP) and contain infusible matter which is insoluble in quinoline (primary) [81]. Presence of

these two factors create serious issues in spinning process. Normally, the spinning is done for

pitches which have softening point above 453 K and before spinning these infusible material

needs to be removed through filtration. Alcaniz-monge et al. pointed out that the presence of

this infusible matter in CTP can distort a continuous spinning process [81, 135]. On the other

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end., to improve the softening points of certain CTP, either heat treatments in air and nitrogen

environment or blending of coal tar and petroleum pitches is done in weight ratio (1:1) [81].

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ACF based CTP can be prepared by activation directly after stabilization (ASF) or through

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common route which is, activated after carbonization (ACFs) of stabilized fibers. ACF
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synthesized by physical activation (carbon dioxide or ammonia) from stabilized Anthracene oil-

based pitch (AOP) were tested as electrode materials in EDLC. The results indicate that the
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functionalization of ACF (through ammonia activation) can enhance the capacitance appreciably

suggesting ammonia activated carbon fibers (N-ACF) to be suitable active materials for EDLC in
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comparison to carbon dioxide activated carbon fibers (C-ACF) [136]. Diez et al. compared the

ACF produced by both routes and suggested ASF to be superior to ACFs and commercial AC in
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terms of BET surface area, electrode characteristics and electrochemical performance [137].
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The general steps in the synthesis of ACF from CTP are pretreatment (filtration, low

temperature heat treatments and/or blending PPs) spinning, stabilization, carbonization and

activation. The general scheme is given in Figure 5.

4.2.2 Petroleum pitch (PP) based ACF

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Petroleum pitch (PP), residue from distillation and heat treatment of petroleum fractions, is the

complex mixture of various aromatic and alkyl-substituted aromatic hydrocarbons [43, 85, 134].

In comparison to CTP-based ACF, PP based ACF contain higher proportion of narrow

microporosity which suggests that microporosity depends on the characteristics and chemical

composition of parent pitch [135].

Steam activated and modified with nitric acid ACF were synthesized from petroleum naphtha

of
cracker bottom oil based pitch at 1173 K for adsorption applications. These ACF (specific

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surface area of 1914 m2/g, micropore volume of 0.73 cm3/g and average pore diameter of 22 Å)

were reported to follow Freundlich model for the adsorption of chromium ions from aqueous

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solutions [138]. Few examples of synthesis parameters, pore size distributions, total surface
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area and applications of PP-ACF are given in Table 3.
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4.3 Phenolic-based ACF

Phenolic-resins are non-natural polymers that can be synthesized with any of the various molar
na

combinations of phenols and aldehydes. However, in this section only phenol and

formaldehyde mixtures are reviewed for ACF production [141]. Novolak and resole are two
ur

well-known phenolic resins for ACF production which could be produced with phenol to
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formaldehyde molar ratios (P/F) of greater and less than 1 in highly acidic and basic reactions,

respectively [142, 143]. The main advantage of phenolic-based ACF is their high carbon content

with low mineral impurities and ash contents [144]. Interestingly, ACF produced from these

resins shows different pore structures ranging from mesoporous structures to microporous

structures depending on the processing conditions applied [143, 145].

19
The manufacturing of phenolic resin (Novolak) based activated carbon fibers is shown in the

Figure 6. Novolak is a thermoplastic and amorphous material, hence curing is required to

increase cross linking and convert fibers into thermosetting. Curing is generally done in acidic

conditions (usually hydrochloric acid) in the presence of a cross linking and hardening agent like

formaldehyde or hexamethylenetetramine (HMTA) at temperature between 313 – 373 K [57,

146, 147]. The infusibility induced in this process makes the carbonization of the fibers possible

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at relatively higher temperatures without losing the shape of the fibers [148].

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Rong Xue et. al. reported the chemical and physical activations of ACF from novolak using KOH

as a chemical activating agent at different temperatures. The results showed significantly higher

-p
specific surface area at 1173 K than physical activation at identical activation temperature. BET
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surface areas of finalized ACF were 1893 m2/g and 939.0 m2/g for chemical and physical

activation, respectively. Furthermore, chemically activated ACF showed better capacitance than
lP

physically activated ACF, when subsequently used in supercapacitor application [149].

na

Oxidation of the spun resin can significantly improve the carbon content in ACF comparative to

non-oxidized precursors. For instance, Hsisheng Teng et al. showed that the carbon yield of
ur

phenol-formaldehyde resin is 33% and 22% with and without oxidation process, respectively

[150]. Oxidization may or may not be the part of ACF production process, as spun fibers can
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directly undergo carbonization [151, 152]. Phenolic resin based ACF doped with silver nitrate

(AgNO3) give antibacterial activity against E. coli and S. Aureus in aqueous solution while

respective CF did not show any antibacterial activities. These ACF were activated physically with

steam at 1173 K resulting in a BET surface area of 2000 m2/g [153].

20
The choice of activation agent significantly influences the porosity and adsorption kinetics thus

dictating the applications of resulting fiber. For example, supercritical water (SCW) and steam

activations of Novoloid based ACF showed different characteristics in terms of the diameter of

fiber, pore-sizes and kinetics of phenol adsorption. Resulting ACF activated with SCW have

micropores in the range of 0.5 – 3.0 nm and showed fast adsorptions of phenol than steam

activated AF which have better surface area with micropores in the range of 0.5 – 2.0 nm [96].

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Few examples of synthesis parameters, pore size distributions, total surface area and

applications of Phenolic resin based-ACF are given in Table 4.

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4.4 Cellulosic-based or Natural-based ACF

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Lignocellulosic biomass could potentially be a huge source of carbon fibers and renewable
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energy. Voluminous amounts of biomass generated each day amounts to millions of tons of
lP

solid waste dumped into landfills [42, 56, 155-157]. Approximately, 40 million tons of inedible

lignocellulosic biomass is generated annually from empty fruit bunch fibers, ramie, corn stover,
na

wheat stems, rice husks, wood shavings, palm leaves and other plant material [158-162].

Though all these biomasses are not in fibrous forms yet can be converted into fibrous form
ur

through processes such as liquefaction, if required [162, 163]. Turning the huge problematic

waste into useful products such as activated carbon fibers has huge appeal [161].
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Lignocellulosic biomass is a generic name for carbon based polymers mostly present in plants,

namely cellulose, hemicellulose and lignin [164]. These natural polymers yield bio-oil, bio-gas

(collectively known as bio-energy) and activated carbons (biochar) when product specific

processing conditions are applied.

21
Current efforts are focused on using Lignocellulosic material as a precursor for ACF production

due to its advantages over other precursors. The fabrication of ACF from lignocellulosic

materials shares similarities in the processing steps with synthetic precursors mentioned

before. The conversion of biomass into high value-added porous ACF requires three vital

processes viz stabilization/pretreatment, carbonization (pyrolysis) and activation (chemical or

physical). The manufacturing process of cellulosic based activated carbon fibers is shown in

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Figure 7.

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Cellulosic fibers are known to have lower carbon content and more hydroxyl groups in their

structure as compared to aforementioned synthetic precursors. These fibers degrade without

-p
fusing or melting, thus, eliminating the need for stabilization or oxidation before carbonization
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step. However, the downside of using lignocellulosic material for ACF production is their lower

carbon content that means low carbon yield – which is a major challenge in ACF fabrication
lP

from lignocellulosic biomass. Treatment methods such as pre-oxidation or pre-treatment of raw

material can increase overall carbon yield. Pre-oxidation is generally carried out with O2, Cl2 and
na

HCl which promotes decomposition at relatively low temperature and enhances carbon yield

[57, 165]. Pre-treatment is mostly carried out by impregnating the fiber or cellulosic material
ur

with the flame retardants viz halides, strong acids, strong bases and Lewis acids. Pre-treatment
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of lignocellulosic material enhances the carbon yield by promoting dehydration and reducing

unfavorable levoglucosan production during pyrolysis [57, 165]. Levoglucosan is an undesirable

byproduct in ACF production and is known to decompose in the presence of air or oxygen [166-

168]. High porosity AC having specific surface area of 1154 m2/g were prepared using combined

process of chemical impregnation followed by oxidation and activation of rice straws. The

22
carbon yield of AC using the combined process was considerably higher in comparison to

carbon yield of AC without peroxidation or direct carbonization [169]. These results dictate the

significance of pre-treatment protocols and chemical activation for high performance porous

AC and ACF production from lignocellulosic material.

Carbonization of lignocellulosic material is undertaken prior to the activation process. The raw

or pre-treated lignocellulosic feedstock undergoes pyrolysis, in inert environment (mostly N 2),

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to enhance the carbon content in the matrix [158]. Carbonization of lignocellulosic precursor is

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carried out at elevated temperature range of 773 – 1173 K resulting in a carbon rich product.

[170, 171]. Lignocellulose material undergoes significant structural changes, weight loss and

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shrinkage at elevated temperatures. At temperatures below 513 K, water is released due to
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desorption (<423 K) and dehydration of cellulosic fragments (423 – 513 K). At elevated

temperatures (>513 K), lignocellulosic material is decomposed through thermal cleavage of

lP

linkages and scission of bonds resulting in emission of carbon dioxide, carbon monoxide, water

and tar [39, 172]. Ioannidou et al. in his review concluded that the carbon content of the char
na

increase while the oxygen and carbon content of the biomass decreases significantly as the

carbonization temperature is increased [173]. Liu et al. studied the pyrolysis of wood-derived
ur

rayon fiber and reported the schematic representation of formation of pyrolysis products such
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as tar [167]. The carbonization of lignocellulosic material is a combination of complex reactions,

and the detailed description of the chemical reactions, mechanisms, structural changes and

pore development during carbonization has been provided by few other researchers [57, 71,

174].

23
The pore development in lignocellulosic based ACF is strongly influenced by the carbonization

temperature, residence time and heating rate. Daud et al. studied the effect of various

carbonization temperatures effect on the pore development of AC and concluded that the

elevated carbonization temperatures result in high micropore volume of the subsequent

activated carbon produced [171]. Similar trends were reported by other researchers with the

fact that the micropore volumes show a maximum value at an intermediate carbon burn-off

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and reduce thereafter [171, 173, 175-177]. This could be due to the coalescence of

micropores into mesopores as the pores tend to grow at elevated temperature and residence

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times. According to McDougall et al., carbonization reduces the volatile content and prepares

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the carbon rich carbonaceous material for subsequent activation [178]. This process introduces

initial porosity through selective elimination of readily available and highly reactive carbon
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compounds [171]. Further activation removes the tar products from the pores and enhances
lP

porosity through pore widening and pore drilling.

Several biological precursors are utilized for the lab scale preparation of ACF such as jute fiber,
na

coconut fiber, flax fiber, oil palm fiber, cotton fiber, silk fiber, hemp, ramie, bamboo and wood

(by liquification) [59, 160, 162, 179-185]. In a typical example, liquefied poplar bark was
ur

converted into fibrous form. The fibers were then cured in formaldehyde and HCl solution
Jo

(37:30 by volume). The cured samples were washed and dried. The dried samples were steam

activated at activation temperatures ranges of 973 – 1173 K for one hour with a steam flow rate

of 4.84 g/min under nitrogen environment. The results indicate that the surface area at 1173 K

was superior to that of lower temperatures. Conversely, the yield lowered from 43.45 % to

14.37 % as the temperature increased from 973 to 1173 K. As the activation temperature

24
increases, the surface area and micropores increase while the yield decreases [186]. Such

trends have been reported by most researchers. On the contrary, the BET surface area of reedy

grass leaves based ACF increased gradually from 690 to 1474 m2/g as the activation

temperature increased from 673 to 773 K and then decreased as the activation temperature

was further increased [187]. This dictates that elevated temperature and prolonged residence

times can cause pores to enlarge and then collapse or coalescence thus decreasing the surface

of
area and micropores. Jian et al. patented the preparation of highly porous lignin based material

through melt spinning, chemical thermo-stabilization by HCl, carbonization at 1473 K and

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subsequent activation of the carbonized material [188]. Similarly, Ruan et al. prepared ACF

-p
through pre-treatment followed by pre-oxidative dehydration, carbonization and finally

activation. The resulting ACF was reported to be highly porous with surface area exceeding
re
2500 m2/g [189]. Details for several ACF preparation variables and the properties of the finished
lP

ACF along with their reported applications have been presented in Table 5.
na
ur
Jo

25
5. Applications

ACF general characteristics like high thermal stability [3], strength, and flexibility, porous

structure controllability enable them to be utilized in various applications like catalyst support

[196], sanitation [197] agricultural and commodities manufacturing [198], adsorbent [199],

supercapacitors [200] and other gas storage applications [201]. Details of important

applications are given below.

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5.1 CO2 adsorption

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Recent global concerns in regard of catastrophic environmental changes, including air pollution,

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global warming are often associated with increasing emissions of CO2 [202-204]. Efforts are
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being made to either decrease CO2 at first place or to reduce it by taking external measures.

Basic strategies in terms of external measures are CO2 capture and sequestration (CCS) process
lP

where CO2 is captured from the existing static sources compressed, injected and stored

underground in deep saline formations [205]. High operational cost, availability and suitability
na

of the storing places of huge amount of captured CO2 are two main concerns in CCS process.

Cost effective potential solutions of CO2 mitigations are absorption, adsorption, cryogenic
ur

distillation, and membrane separations.[206]. ACF with high adsorption capacities than porous
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silicas, zeolite, porous alumina’s and metal-organic compounds for CO2 are being synthesized.

Shen et. al. revealed that Nitrogen functional groups and the basic sites present on the surface

of KOH activated PAN based ACF are responsible for increased rates of adsorption, which made

the surface CO2 friendly [202]. Nitrogen and N – functional groups evenly distributed over the

26
matrix and the bulk of the ACF positively influenced the adsorption of CO2. A detailed study

revealing the effects of N doping on the surface and within matrix of ACF using pitch (oil-based)

and blend of either melamine–formaldehyde or urea–formaldehyde resin and pitch,

respectively, is done by Diez. Maximum uptake was determined to be 151 mg g-1 at infinite time

and 67 mg g-1 at 100 s [204].

C – H groups on ACF surface produced favorable results in the study conducted by Byong Chol

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Bai et. al. with 112% better CO2 adsorption, 1.61 comparative to 0.76 mol/kg, of liquid-oxidized

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ACF than otherwise [206]. Micropores (1.0 nm) at the surface of ACF proved to be the suitable

size for CO2 molecular level adsorption and hence improved sorptive results are achieved with

-p
highest sorption of 250 mg g-1. Concentration of the KOH in chemical activation process dictates
re
the pore size distribution on the surface of produced ACF and 3:1 (KOH/ACF) is the optimum

ratio at STP in the given case. CO2 adsorption capacities of these commercially available ACF are
lP

determined by Lee and Park, the concluding capacity was determined to be as high as

250 mg g-1 [203].

na

Hence, influencers like rapid rate of adsorption, induced CO2-philic nature by doping ACF with N

containing compound, C – O functional groups, and molecular size consistent pores

ur

development at the surface and bulk of carbon matrix, selective physisorption, easy
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regenerations, convenient handling of ACF are suggesting positive prospects as an adsorbent

for CO2. CO2 adsorption capacities of ACF produced from various precursors are given in Table 6

and schematized in Figure 8.

27
5.2 VOC adsorptions

Volatile organic compounds (VOCs) have high vapor pressures owing to their high volatility at

STP. VOCs have adverse effects on environment such as depletion of ozone layer and formation

of photochemical smog. Moreover, their exposure to human body can cause severe health

problems ranging from eye irritation to cancer [210-213]. Owning to their inherent importance

of
and unavoidability – being the compulsory part of industrial off-gases and household chemicals

namely paints, pharmaceuticals, degreasers, varnishes, organic solvents, chemical cleaners,

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petrochemical, printing industry, wastewater treatment process VOCs admittance to human

-p
ecosystem particularly indoor emissions can’t be mitigated at production level [214-216]. The

most commonly encountered VOCs are benzene, toluene, xylene, (BTX) organic compounds
re
such as acetone, ethanol and other chlorinated hydrocarbons. Several efforts have been made

to eliminate VOCs particularly from contained environment and various techniques have been
lP

proposed and utilized in this regard. The adsorption of VOCs through ACF is demonstrated in

the Figure 9. Keen studies were done to control VOCs using condensation, adsorption, thermal
na

and catalytic oxidation [217]. At high concentrations of VOCs the Adsorption process depends

only on the pore volume i.e. macropores and not on the microporosity and nature of the
ur

adsorbate whereas, at low concentrations its adsorption depends on microporosity and

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polarization of the specific adsorbate to be used [212, 218]. Table 7 presents ACF, and their

adsorption capacities for VOCs and dyes removal.

28
5.3 Wastewater Treatment

Refineries, petroleum industries and textile industries generate sheer quantities of wastewater

containing high concentration of oil, organic wastes and dyes which is one of the major

concerns to environment in general and water bodies in particular [226-229]. Textile industry,

in itself, is one of the largest producers of toxic wastewaters containing dyes capable of causing

carcinogenic and mutagenic effects [230-233] and has been classified as “most polluting” owing

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to the effluent concentration and the immense volume of wastewater discharged [234, 235].

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Approximately, 0.2 million tons of dyes are estimated to end up as effluents out of 0.7 million

tons of synthetic dyes being produced annually [236, 237]. Wide variety of pigments and dyes

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employed in worldwide industries results in high variations in effluent waste water
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concentration from application to application making effluent treatment very complex,

challenging and virtually impossible without the use of sophisticated instrumentation and
lP

experienced personals [237-239]. Textile waste includes various toxic pollutants such as dyes

and surfactants that are highly resistant to biodegradation and thus must be removed before
na

disposal to ensure aquatic life safety, mitigation of pollution, adherence to environmental

legislations and maintaining quality of water bodies [235, 237, 240].

ur

Several techniques are being utilized to treat wastewaters bearing organics materials e.g.
Jo

textile wastewater including, but not limited to, filtration, incineration, adsorption, biological

treatment, advanced oxidation processes, Fenton process, heterogeneous photocatalysis, and

photoelectrochemical process. These processes have the potential to treat organic wastes and

dyes quite efficiently but are quite expensive, complex and are not completely environment

29
friendly [241-249]. Adsorption has been termed as one of the most suitable method for

removal of organic materials (and other pollutants such as heavy metals) from aqueous

solutions as it binds the pollutant within its solid matrices without destroying them [241, 250-

253]. Many cheap adsorbents have been reported in literature for wastewater treatment

particularly heavy metals, dyes and organics, yet their lower adsorption capacity and lower

adsorption rate hinder their commercialization [254-260]. ACF have the potential to be

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considered as one of the most promising adsorbent in terms of environment friendliness and

cost effectiveness due to their excellent intake capacity, high surface area and high contact

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efficiency [261, 262]. Mechanism of waste water treatment using ACF is illustrated in Figure 10.

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ACF can be utilized as an excellent adsorbent materials because of their smaller pores (10 -

40µm) and hence better pores to surface area ratios making them the good choice for the
re
removal of organics, heavy metals and in some cases VOCs from water, as indicated by research
lP

studies [261]. Basic phenomena involve sorption of the oil at the porous surface of ACF.

Sorption is in turn governed by various factors like pH, contact time, initial concentration of the
na

impurity, and temperature.

The adsorption of organics particularly dyes on the ACF mainly depends on ACF pore size
ur

distribution. Microporous ACF are mainly advantageous for low sized organics adsorption
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however for dyes, which are mostly fairly sized, mesopores have imperative influence on

adsorption capacities of dyes as compared to micropores. In a typical example, the adsorption

of acidic, basic and direct dyes on highly porous pitch-based steam-activated carbon fibers was

studied in terms of pore size and surface charge of ACF and dye molecule size. The results

indicate that the dye adsorption on ACF is greatly influenced by pore size of ACF, steric size of

30
dye molecule, surface charges of ACF and the electrostatic interaction between the adsorbent

and the adsorbate. Hsiu-Mei et al. studied the adsorption characteristics of Chrysophenine and

Orange II on ACF and sludge adsorbent and concluded that the large-sized dye molecule

transport into the microporous ACF was inhibited resulting in low adsorption capacities as

compared to adsorption capacities of mesoporous adsorbents. The results indicate that

adsorbent pore size distribution in comparison to the absorbate molecule size is imperative to

of
the adsorption capacities. Similar results have been reported by few other researchers. Table 7

presents ACF, and their adsorption capacities for VOCs and dyes removal.

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5.4 Energy

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ACF and other advanced carbon materials are under immense focus for energy storage
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applications as they are promising materials for the fabrication of electrochemical double layer
lP

capacitors (EDLC), electrodes, standby power systems, portable electronics, flexible and

wearable sensors, telecommunication devices, and smart clothes [137, 263-269]. EDLC, also
na

termed as super capacitors, are known to meet high power demands in miniaturized electronics

[268]. Activated carbon fibers are frequently used in the fabrication of carbon-based
ur

supercapacitors as an active electrode material due to their high-power density, fatigue

endurance, high surface area, low cost and ease in scalability [137, 270, 271]. These fiber-
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shaped electrodes are typically fabricated as composites of electrochemically active materials

and effective fibrous supports for their applications in EDLC. The energy storage on EDLC is

shown in the Figure 11. In a typical example, activated carbon fibers were grafted by

mesoporous carbon and used as an electrode material in the E-Fenton process for brilliant red

31
X3B degradation. The results indicate that such novel ACF@OMC electrodes have enhanced

electrical conductivity, excellent stability and can be used effectively in E-Fenton process for

organic degradation [272]. Li et al. reported the fabrication of flexible fiber SC using composite

of ACF and Manganese MnO2@ACF as a composite electrode. The resultant SC demonstrated

the maximum capacitance, energy density and power density of 410 mF/cm 2 at 0.1 mA/cm2, 36

µWh/cm2 and 726 µW/cm2, respectively [267].

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Several factors such as specific surface area, pore size distribution, pore structure, surface

ro
chemistry and functional groups influence the specific capacitance of the carbon-based

electrodes [273]. Numerous studies have investigated the influence of these factors on the

-p
EDLC performance [273-276]. Lin et al. reported that the pore size range of 0.5 nm – 2 nm is
re
optimal for double layer formation in aqueous electrolytes [277]. Micropores contribute to the

double-layer capacitance while mesopores facilitate good electrolyte transport for high energy
lP

densities [274, 278]. Thus, well-control over pore size distribution and optimization of micro to

mesopores ratio is vital for fabrication of EDLC providing high energy densities and enhanced
na

capacitive performance [279, 280]. Several studies have shown that the presence of functional

groups, such as nitrogen and oxygen functionalities, can enhance the capacitance of EDLC by
ur

improving pseudo-Faradaic reactions and carbon wettability of the porous carbon electrodes
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[281-283]. It is interesting to state that the pseudo capacitance from carefully selected

functional groups can contribute to over 22% of the total capacitance of the EDLC [282, 283].

EDLCs have been reported to provide higher energy and power densities than dielectric

capacitors and batteries, respectively. However, the energy density of EDLC is lower than that

32
of lithium ion battery [284]. Furthermore, the cost of ACF based EDLC is comparatively high

[268]. Thus, the key challenge towards the practical applications of ACF based EDLC is the

development of low cost ACF with high power and energy densities [285]. The use of low-cost

renewable lignocellulosic material for ACF production and subsequent EDLC fabrication is a

promising route in this context [282, 284, 286]. Thus, unique advantages of ACF over other

forms of AC such as higher flexibility, adsorption characteristics and textural properties, ACF has

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been promoted to be the most widely researched strategic material for energy storage

applications [160, 287-290].

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6. Summary and Discussion

-p
Several efforts have been made by researchers to quantify carbon and its activation under a
re
range of parameters [22, 291-293]. Owning to its vast end usage and valuable nature carbon
lP

has been activated in different shapes among them most common structures are powdered

[294], granular [295, 296], monolithic [297], nanotubes [298, 299] and fibrous [300]. Powdered
na

activated carbon (PAC) are best adsorbents where fast rate of adsorptions kinetics is required,

however pressure losses in gas adsorption and handling difficulties in liquid adsorption make
ur

granular activated carbon (GAC) a preferable choice for gas adsorption despite of their low

adsorption kinetics [301]. Pretreated fibrous carbon when processed in either physical or
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chemical activation conditions turn into activated carbon fiber (ACF) which can be felted into

clothes or other shapes depending upon end user applications [301]. Versatility in shape, rich

microporous structure easy handling, fast adsorption kinetics and multifold regenerations,

make ACF one of the most useful recent development in activated carbon family [71]. It can be

33
used directly in protective clothing [302], liquid [179] or gas phase applications and other

intermediatory uses such as catalytic support [209, 303, 304].

ACF offers large specific surface area, controllable pore size distribution, fast adsorption

kinetics, high adsorption capacities, rapid regeneration, shape stability and longer life span than

AC [45, 305, 306]. Carbon fibers have excellent mechanical properties, high thermal and

electrical conductivities and low thermal expansion coefficient making them a suitable

of
structural materials [45]. For similar operational conditions, ACF have several advantages over

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conventional activated carbon forms in liquid and gas applications such as adsorption, gas

removal and catalytic processes [305-307]. The microporous structure of ACF with narrow pore

-p
size distribution allows them to have high specific surface area, enhanced adsorption capacities
re
and fast kinetics [45]. In addition, ACF can be easily processed into a great variety of fabric

forms such as felt, paper, cloth and honeycomb due to their compactness, light weight, peculiar
lP

fibrous structure with diameter ranging between 10-40 µm, easy moldability, and lower

pressure drops [307]. Moreover, the use of ACF in liquid or gas applications offers great
na

flexibility and low hydrodynamic resistance at elevated flow rates [307]. The narrow pore size

distribution of ACF can be tailored to synthesize ACF with different pore sizes that can be
ur

adapted for specific applications in separation processes, water treatment, air sanitation, gas
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capture, solvent recovery and as catalysts and catalyst supports in catalytic processes for

enhanced selectivity. For instance, ACF-Polyaniline composite was mentioned to be potentially

an ideal capacitive deionization (CDI) electrode material having higher ion-electrosorption

capacitive efficiency and robust stability compared with other carbon forms [308, 309].

34
Owing to these characteristics, ACF is getting ever increasing attention in applications such as

adsorption, energy, gas removal and filtration. The preparation, characterization, applications

advantages and limitations of ACF have been reported in several studies. The production of

ACF is done through carbonization followed by activation (physical or chemical) during which

surface area increases and porosity develops. The chemical activations have several advantages

over physical activation such as low activation temperature, high char yields and reduced

of
reaction times for sample activation. The main disadvantage of chemical activation is the use of

corrosive chemicals and the requirement of a thorough washing step to remove these corrosive

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chemicals.

-p
Several types of precursors have been used for ACF production over the recent years. Use of
re
each precursor offers a unique set of advantages and limitations for the prepared ACF. An ideal

precursor possesses a fibrous structure, high carbon contents and low lignin and inorganic
lP

contents. Materials like cotton stalk, jute fiber and bamboo are considered valuable precursors

to produce ACF as they reduce processing steps like stabilization, densification while improving
na

microporosity and mechanical strength of final product. Non-natural precursors based ACF

show good properties, but their non-renewability make them a less desirable choice.
ur

Precursors such as PAN, phenolic, pitch and rayon are mainly petroleum derived products and
Jo

thus have several limitations particularly related to being non-renewable, high processing costs

and non-environment friendly [11]. Low cost ACF are being produced from renewable biomass

rich in lignocellulosic, hemicellulosic and lignin contents generated either from soil such as oil

palm fibers, jute fibers and coconut fibers or industrial waste such as wheat stems, rice husks

35
and wood shavings. These materials are ecofriendly, easily available and low and have low

processing costs [179]. Other unique characteristics of lignocellulosic precursors are low cost,

biodegradability, high thermal conductivity, high purity, mechanical flexibility, high

microporosity of prepared activated carbons and commercial availability [310]. Nonetheless,

despite the unique characteristics and advantages, the lignocellulosic materials are not yet

considered as a good precursor for ACF fabrication due to their relatively low char yield, low

of
degree of orientation and discontinuous fiber filament structure [42]. Pre-treatment of

lignocellulosic material before carbonization has shown to increase the carbon yields to an

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acceptable limit. Furthermore, lignocellulosic-based ACF cannot be utilized in high-performance

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composite materials due to their relatively low tensile strength (~ 1000 MPa) [311]. Thus,

currently the foremost uses of lignocellulosic based ACF are in energy storage, water and air
re
treatment applications and gas storage.
lP

PAN-based precursors are quite dominant among other precursors for ACF production owing to

their higher carbon yield, higher melting point, fast pyrolysis rate and exceptional strength as
na

compared to other precursors [80]. Major drawbacks of PAN-based ACF are their high cost, use

of toxic chemicals in production, low surface area, porous volume and reduced tensile strength.
ur

Comparatively, Kynol-based ACF is superior to PAN-based ACF in surface area and equivalent to
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PAN-based ACF in tensile strength [5]. A detailed review on the mechanical properties of ACF

from different precursors has been provided by Li et al. [312].

Phenolic-based ACF are preferred over pitch-based and lignocellulosic-based ACF as they are

known to have high thermal stability, high corrosion resistance and high thermal insulation.

36
Traditionally, phenolic resins are produced through non-renewable raw materials aka. phenol

and formaldehyde. Recent studies have been focused on finding renewable substitutes from

non-fossil sources, such as biomass, for these non-renewable raw materials [313, 314].

Consequently, several studies have established that condensed tannins and gallic acid from bio-

sources could be used for the synthesis of phenolic resins and bio-based epoxy resins,

respectively [42, 315, 316].

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Hunt for cheap raw materials should be extended since only a few natural cellulosic precursors

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have been reported since the recovery of ACF [317]. Process cost can be managed by utilizing

the byproducts generated in the manufacturing of ACF, particularly if bio-gas would be directed

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to other useful purposes [5]. The scope of its applications could be broadened by applying ACF
re
to replace the non-degradable commonly used products like plastic shopping bags, containers,

plastic body devices and insulations. Moreover, research can be focused on the separation or
lP

recycling of rare earth elements (REE) by inducing charge on the surface of ACF, by direct

adsorption desorption methods or by improving the rare earth elements philic (REEsP)
na

characteristics of ACF by making metalloid composites.

ur

Traditional data storing and recording appliances could be replaced with delicate ACF made

devices owing to its electrical properties [140]. Furthermore, antibacterial properties of ACF
Jo

could be handy in medical applications especially as a substitute of conventional bandages,

tissue and wound stitching, veins and arteries connections and dedicated dosage (medicines)

transport within the human body [153]. In other words, keeping the versatile nature of ACF in

view more rigorous applications need to be discovered.

37
Conversion of biomass generated annually into ACF has several-fold advantages. Voluminous

amounts of biomass generated each day amounts to millions of tons of solid waste dumped

into landfills. The interesting fact that large scale human management of waste biomass can

impact the Earth’s climate significantly and can potentially offset one seventh of current GHG

emissions is exceptionally appealing towards large scale ACF production from sustainable

biomass precursors. Apart from means of mitigating climate change, ACF production also

of
results in substantial amounts of energy in the form of bio-oil and bio-gas collectively known as

bio-fuel. The combustion of bio-fuel to meet the energy demands of ACF production in a

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combined pyrolysis-combustion process can lead to enhanced bio-economy and sustainability

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of the process. In-depth study and understanding of feed stock characteristics, pyrolysis

parameters and atmospheric emissions is crucial to establish correlations between process

re
parameters and develop a set of optimum conditions for biomass conversion into ACF and bio-
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fuel for effective renewable energy generation and waste management.

Though it is of no doubt that the final raw material and process conditions for ACF production
na

depend on the end-use application of the ACF. Yet the main challenges come from cost

effectiveness, low carbon footprints and energy efficiency. ACF from lignocellulose has added
ur

advantages of low cost and low carbon footprints. These aspects necessitate the advancement
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of present knowledge and development of new technologies with robust and sustainable

supply chains.

7. Conclusion and Future Prospects

38
Activated carbon fibers (ACF) can be synthesized through thermochemical processes

(stabilization, carbonization and activation) in which the precursors range from PAN, phenolic,

pitch and lignocellulosic material capable of producing high surface area products terms as ACF.

The production of ACF from lignocellulosic material has been proved to be more economical,

advantageous and environment friendly as compared to ACF from other precursors due to

several reasons including, but not limited to, the use of renewable precursors, reduced

of
processing steps and costs, and conversion of waste material (lignocellulose) into useful

products (ACF). This in turn could help in reducing the environmental problems related to waste

ro
disposal and hazardous material emissions to the environment.

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The use and application of ACF from lignocellulose on industrial as well as small farm scales
re
pose substantial challenges including, but not limited to, lack of knowledge about suitable

biomass feedstocks, high variations in bio-fuel properties, comparison between variety of

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biomass relating to their yield, characterization of products, soil amendment benefits and

capital costs. These factors, along with the variations in biomass quality and chemical
na

composition, present a problematic system for the effective, cost-efficient and environment

friendly production of ACF and energy from biomass. Very few reports have been published on
ur

ACF production from waste biomass and its significance in terms of industrial applications, bio-
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energy production, particulate and gas capture, improving soil quality factors, carbon

sequestration and climate change abatement [5, 11]. Thus, in-depth study and understanding

of feed stock characteristics, pyrolysis parameters and atmospheric emissions is crucial to

establish correlations between these parameters and develop a set of optimum conditions for

39
biomass conversion into ACF for effective renewable energy generation and carbon

sequestration.

Conflict of Interest

The authors declare no conflict of interest.

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re
lP
na
ur
Jo

60
Figure Captions (JAAP 104715)

Figure 1. Venn Diagram demonstrating the ACF classification in carbon materials. Adapted from

[11]

Figure 2. Number of Publications related to ACF since 1995

Figure 3. Synthesis and applications of ACF

of
Figure 4. Generalized Production Process of PAN based ACF

Figure 5. Generalized Production Process of Pitch based ACF

ro
Figure 6. Generalized Production Process of Phenolic based ACF

-p
Figure 7. Generalized Production Process of Cellulosic (and biomass) based ACF
re
Figure 8. Schematic Diagram of CO2 Capture by ACF
lP

Figure 9. Schematic Diagram of VOC capture by ACF

Figure 10. Schematic Diagram of Dye Adsorption from wastewater by ACF

na

Figure 11. Schematic Diagram of ACF use in EDLC Fabrication

ur
Jo

61
Jo
ur
nal
Pre
-p
ro
o f
Jo
ur
nal
Pre
-p
ro
o f
Jo
ur
na
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re
-p
ro
o f
Jo
ur
nal
Pre
-p
ro
o f
Jo
ur
nal
Pre
-p
ro
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Jo
ur
nal
Pre
-p
ro
o f
Jo
ur
nal
Pre
-p
ro
o f
Jo
ur
nal
Pre
-p
ro
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Jo
ur
nal
Pre
-p
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o f
Jo
ur
nal
Pre
-p
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Jo
ur
nal
Pre
-p
ro
o f
Table 1: Characteristics of different activated carbon forms

Activated
Characteristics Advantages Disadvantages
Carbon

Slow kinetics

Bad selectivity

Limited design flexibility

of
Granular, large
Granular Low cost Working capacity < 100%
particle size

ro
Relatively low accessible

porosity

-p complicated regeneration
re
Limited design flexibility

Unsuitable for filtration

lP

systems

Small particle Increased accessible porosity High pressure drop in flow

na

Powdered
size relative to GAC systems

Cause of secondary pollution

ur

when disposed
Jo

Complicated regeneration

Higher adsorption rates

Fiber- Fibrous
High accessible porosity High cost
shaped structure
High surface area

62
 Improved contact

efficiencies with media

Adequate design flexibility

Easy regeneration

(particularly thermal)

of
ro
-p
re
lP
na

Table 2: The precursors, carbonization temperature, activation temperatures and characteristics of PAN-

based ACF
ur

Activation Volume
Jo

BET Yiel
Tim Micr Referen
Material TC Activati TA Surfac Vt d Application
e o ce
on agent e Area

K K Hr m2/g cc Cc %

63
 973
Polyacrylonitr 722.9 0.26 0.32
127 –
ile /pitch Steam 1 – – – - - [121]
3 117
blends 1877 0.55 1.11
3

Potential

Textile PAN 117 Carbon 127 50 electrochemi

1260 0.53 0.59 - [94]
fibers 3 dioxide 3 min cal

of
applications

ro
973 0.25
Electrospun 722.9 0.32
127 – 8–

-p
PAN/ pitch Steam 1 – 4– - - [121]
3 117 0.54
fiber 1877 1.11
3 8
re
873 923 Catalytic
lP

– – 0.5 412 – 14 – activity for

-
PAN Steam - [119]
127 112 –5 670 54 sulfur dioxide
na

3 3 conversion

873 873 Catalytic

– – 30 271 – 82 – activity for

ur

-
PAN KOH - [119]
107 107 min 3388 38.4 sulfur dioxide
Jo

3 3 conversion

Pitch- 107 0.22 Carbon

Carbon 1– 366 –
phenolic resin 923 3– – - - dioxide [122]
dioxide 1.5 424
composites 117 0.21 capture

64
 3

Activated

pitch – 112 819 –

1 0.43 - -
phenolic resin 3 925

composites

PAN – 0.07
107 140 –
phenolic resin 2 – - -

of
3 245
composite 0.13

ro
-p
re
Table 3: The precursors, carbonization temperature, activation temperatures and characteristics of Pitch

(petroleum and coal tar) based ACF

lP
na
ur
Jo

65
 Surf

Carbonizati ace
Activation Volume
on Are
Yie
a
ld Applicati Refer

of
Precursor Ti
Mi on ence
TC Activat TA m BET Vt

ro
cro
ion e

K
agent
K Hr
-p
m2/

g
cc cc %
re
Till
lP

50

11 % 109 00. 0.6

Steam
na

Anthracene oil- 23 bu 8 46 2
SO2
based pitch rn
1143 catalytic [139]
ur

(isotropic) (Co- off

oxidation
doped) KOH
Jo

(KOH/C 11 129 0.5 0.6

1
F =7/1 23 4 6 0

wt.)

Anthra One step 11 Till 145 0.6 Electrode

ACF [136]
cene carbonizatio 73 66
50 4 18 material
oil- n/Activation CO2 % in EDL

based bu capacitor

pitch rn

(AOP) off

N- 11 0.3
NH3 0.5 891
ACF 23 77

of
NaOH 110 0.4 0.5 electrode
1173 33
Coal-based (NaOH/ 11 1 1 2 s in

ro
1 [137]
pitch Direct fiber 73 246 0.8 1.3 Supercap
17
activation 3/1)

10 -p
0 5 4 acitors
re
152 0.5 0.6
mi
0 8 1
lP

20
175 0.6 0.7
na

mi Specific
Pitch-based 11 0 7 3
- Steam n capacitan [140]
(CF) 73
ur

30 ce
265 0.9 1.1
mi
Jo

0 8 5
n

40 323 0.8 1.8

mi 0 3 9

67
 Jo
ur
na
n

68
lP
re
-p
ro
of
Table 4: The precursors, carbonization temperature, activation temperatures and characteristics of

Carbo Surfa
Materi Yiel Refere
nizati Activation ce Volume Application
al d nce
on Area

of
ro
-p
re
lP
na
ur
Jo

phenolic resins based ACF

69
 Activati Tim Mic
TC TA BET Vt
on e ro

K agent K Hr m2/g cc cc %

10 280 53 Antibacteri

al

Novoly properties

of
tic-type with Ag
1273 Steam 1273 - - [153]
phenol 60 1940 21 doping and

ro
resin potentials

-p for water

purifying
re
0.26 0.2
super
lP

903 – 1 – 499 – 9 – 72 –
Novoloi critical
1023 30 1145 0.52 0.6
d water Adsorption
na

4 54
(phenol 973 - of phenol [96]
0.31 0.3
ic onto ACF
ur

903 – 1 – 581 – 5 – 21 –
fibers) Steam
1023 30 1490 0.71 0.7
Jo

5 82

Phenoli KOH:CF 873 – 738 – 0.37 0.3 electroche

1123 1 - [154]
c fibers (4:1) 1173 1893 0 – 90 – mical

70
 0.72 1.0 supercapaci

7 0 tors

0.46 0.5
CO2 1173 2 939
1 34

of
ro
-p
re
lP
na
ur
Jo

71
Table 5: The precursors, carbonization temperature, activation temperatures and characteristics of

Cellulosic-based or Natural-based ACF

Activation Volume

BET
Tim Micr Yield Referenc
Material TC Activatio TA Surfac Vt Application

of
e o e
n agent e Area

ro
K K Hr m2/g cc cc %

Phenol 973 14.3

-p
0.38 Carbon
liquefied – 716.4 7–
-
Steam 1 – molecular [186]
poplar 117 – 1483 43.4
re
0.70 sieve
bark 3 5
lP

673
0.43 0.77 34.9
Ramie – 1– 1597 –
-
ZnCl2 – – – EDLC [160]
na

fibers 102 2 2087

0.60 1.08 38.1
3
ur

Ceiba
Methylene
pentandra 10 – 0.28
431 – blue removal
Jo

-
(L.) 973 Steam 973 50 – [190]
753 from aqueous
Gaertn. min 0.62
solution
(kapok)

H2SO4
Oil palm 673 117 1 632 – 0.24 0.26 18.9 Adsorption [191]

72
empty Carbon 3 990 – – –

fruit dioxide 0.39 0.42 29.2

bunch

fiber

Low High energy

sulfonated 112 112 density

NaOH 0.5 1027 [54, 192]
alkali 3 (S) 3 supercapacito

of
lignin rs

ro
Low High energy

sulfonated 112 density

-p
KOH 0.5 1407 [54, 192]
alkali 3 supercapacito

lignin rs
re
potassiu
lP

dihydroge
p-nitroaniline
na

n
adsorption
phosphat
Cotton 112 20
873 1520 0.89 1.20 - from aqueous [193]
e solution
ur

stalk 3 min
solutions
(pre-
Jo

onto ACF
treatment

Steam

73
 ZnCl2

102 102 30 0.16 0.52

Steam +
527
3 3 min 4 4
Carbon

dioxide

ZnCl2
117 117 30 0.41 1.97
Cotton 2053 Adsorption
Carbon

of
3 3 min 3 3 [194]
Stalk application
dioxide

ro
Sulfuric

acid
112

3
Steam +
112

3
20

min
309
0.04

4
-p 0.34

4
re
Carbon

dioxide
lP

Cotton
p-nitroaniline
Stalk
na

adsorption
560 9 0.08 37.9
(Microwav
- ZnCl2 794.84 0.63 from aqueous [195]
W min 3 2
ur

e assisted
solutions
chemical
onto ACF
Jo

activation)

H3PO4 Adsorption of
640 10
Cotton 773 Microwav 1370 - 0.98 40 methylene [56]
W min
e assisted blue onto ACF

74
 of
Table 6: ACF prepared from various precursors and their use in carbon dioxide capture

ro
Surface area
Precursor Precursor type Activation agent Gas Storage capacity Reference

-p
(m2/g)

Poly-acrylonitrile

re
Synthetic KOH 2231 CO2 4.4mmol/g [202]
PAN

Commercially

available chopstick- N/A

lP
KOH 2180 CO2 250mg/g [175]
na
like ACF

Phenolic resin
ur

Synthetic CO2 998 CO2 0.416 mmol/g [207]

composite
Jo

Anthracene oil-
Synthetic KOH 909 CO2 67 mgCO2/g [204]
based pitch

75
Poly-acrylonitrile
Synthetic KOH 979 CO2 1.61mol/kg [206]

of
(PAN) fibers

ro
Natural silk fibers Natural KOH 3000 CO2 4.8mmol/g [208]

N-doped carbon

-p
nanotubes (CNs)
Synthetic N/A 886 CO2 1.92mmol/g [209]

re
grafted polyamide

(PAN) based ACF

lP
na
ur
Jo

76
 Table 7: ACF prepared from various precursors and their use in VOC and dyes removal

of
Activation Surface area VOCs, Dyes and other Adsorption
Precursor Precursor type Reference

ro
agent (m2/g) organics capacity

1,1-DCE 31.3mg/g

-p
Polyacrylonitrile TCE 52.5mg/g
Synthetic N/A 1075 [219]

re
(PAN) PCE 57.0mg/g

1,1,2-TCA 33.8mg/g

lP 1,1-DCE

TCE
37.5mg/g

62.5mg/g
na
Phenolic resin Synthetic N/A 1513 [219]
PCE 81.0mg/g

1,1,2-TCA 40.0mg/g
ur

MEK 250mg/g
Viscos rayon Synthetic N/A 1460 [220]
Jo

non-polar benzene ~290mg/g

polymeric fibres n-Butane ~4.6 mmol/g

Synthetic Steam 1306 [212]
(Nomex ) n-hexane ~4.0 mmo/g

77
Phenolic resin Synthetic N/A 1027 2-Chloroethano l 0.61g/g [221]

of
Kynol novoloid
Synthetic N/A 2220 Toluene 4.6mol/kg [222]
(phenolic) fibers

ro
Hemp (Cannabis
Natural N/A 1142 Acid blue 9 28.75 mg/g [223]

-p
sativa L.)

Oxytetracyclinehydroc

re
cotton linter fibers Natural NaOH 2143 1340.82 mg/g [62]
hlorid (OTC)

Cotton

Kenaf fibers
Natural

Natural
lP
N/A

K2HPO4
2060

493
Methylene blue

Phenol
597 mg/g

140.84 mg/g
[224]

[225]
na
p – Nitrophenol 136.99 mg/g
ur
Jo

78