Nanofiber

Example of a cellulose nanofiber network.

Nanofibers are fibers with diameters in

the nanometer range. Nanofibers can be
generated from different polymers and
hence have different physical properties
and application potentials. Examples of
natural polymers include collagen,
cellulose, silk fibroin, keratin, gelatin and
polysaccharides such as chitosan and
alginate.[1][2] Examples of synthetic
polymers include poly(lactic acid) (PLA),
polycaprolactone (PCL), polyurethane
(PU), poly(lactic-co-glycolic acid) (PLGA),
poly(3-hydroxybutyrate-co-3-
hydroxyvalerate) (PHBV), and
poly(ethylene-co-vinylacetate)
(PEVA).[1][2] Polymer chains are
connected via covalent bonds.[3] The
diameters of nanofibers depend on the
type of polymer used and the method of
production.[4] All polymer nanofibers are
unique for their large surface area-to-
volume ratio, high porosity, appreciable
mechanical strength, and flexibility in
functionalization compared to their
microfiber counterparts.[1][2][5]

There exist many different methods to

make nanofibers, including drawing,
electrospinning, self-assembly, template
synthesis, and thermal-induced phase
separation. Electrospinning is the most
commonly used method to generate
nanofibers because of the
straightforward setup, the ability to
mass-produce continuous nanofibers
from various polymers, and the capability
to generate ultrathin fibers with
controllable diameters, compositions,
and orientations.[5] This flexibility allows
for controlling the shape and
arrangement of the fibers so that
different structures (i.e. hollow, flat and
ribbon shaped) can be fabricated
depending on intended application
purposes.

Nanofibers have many possible

technological and commercial
applications. They are used in tissue
engineering,[1][2][6] drug delivery,[7][8][9]
cancer diagnosis,[10][11][12] lithium-air
battery,[13][14][15] optical sensors[16][17][18]
and air filtration.[19][20][21]

History of nanofiber
production
Nanofibers were first produced via
electrospinning more than four centuries
ago.[22][23] Beginning with the
development of the electrospinning
method, English physicist William Gilbert
(1544-1603) first documented the
electrostatic attraction between liquids
by preparing an experiment in which he
observed a spherical water drop on a dry
surface warp into a cone shape when it
was held below an electrically charged
amber.[24] This deformation later came to
be known as the Taylor cone.[25] In 1882,
English physicist Lord Rayleigh (1842-
1919) analyzed the unstable states of
liquid droplets that were electrically
charged, and noted that the liquid was
ejected in tiny jets when equilibrium was
established between the surface tension
and electrostatic force.[26] In 1887, British
physicist Charles Vernon Boys (1855-
1944) published a manuscript about
nanofiber development and
production.[27] In 1900, American
inventor John Francis Cooley (1861-
1903) filed the first modern
electrospinning patent.[28]

Anton Formhals was the first person to

attempt nanofiber production between
1934 and 1944 and publish the first
patent describing the experimental
production of nanofibers.[23] In 1966,
Harold Simons published a patent for a
device that could produce thin and light
nanofiber fabrics with diverse motifs.[29]

Only at the end of the 20th century have

the words electrospinning and nanofiber
become common language among
scientists and researchers.[22][23]
Electrospinning continues to be
developed today.

Synthesis methods
Many chemical and mechanical
techniques for preparing nanofibers
exist.

Electrospinning
Diagram of a general set-up of electrospinning.

Taylor cone from which jet of polymer solution is

ejected.

Electrospinning is the most commonly

used method to fabricate
nanofibers.[30][5] [31] The instruments
necessary for electrospinning include a
high voltage supplier, a capillary tube
with a pipette or needle with a small
diameter, and a metal collecting screen.
One electrode is placed into the polymer
solution and the other electrode is
attached to the collector. An electric field
is applied to the end of the capillary tube
that contains the polymer solution held
by its surface tension and forms a
charge on the surface of the liquid. As
the intensity of the electric field
increases, the hemispherical surface of
the fluid at the tip of the capillary tube
elongates to form a conical shape known
as the Taylor cone. A critical value is
attained upon further increase in the
electric field in which the repulsive
electrostatic force overcomes the
surface tension and the charged jet of
fluid is ejected from the tip of the Taylor
cone. The discharged polymer solution
jet is unstable and elongates as a result,
allowing the jet to become very long and
thin. Charged polymer fibers solidifies
with solvent evaporation.[5][32] Randomly-
oriented nanofibers are collected on the
collector. Nanofibers can also be
collected in a highly aligned fashion by
using specialized collectors such as the
rotating drum,[33] metal frame,[34] or a
two-parallel plates system.[35]
Parameters such as jet stream
movement and polymer concentration
have to be controlled to produce
nanofibers with uniform diameters and
morphologies.[36]
The electrospinning technique
transforms many types of polymers into
nanofibers. An electrospun nanofiber
network resembles the extracellular
matrix (ECM) well.[5][37][38] This
resemblance is a major advantage of
electrospinning because it opens up the
possibility of mimicking the ECM with
regards to fiber diameters, high porosity,
and mechanical properties.
Electrospinning is being further
developed for mass production of one-
by-one continuous nanofibers.[37]

Thermal-induced phase
separation
Thermal-induced phase separation
separates a homogenous polymer
solution into a multi-phase system via
thermodynamic changes.[1][6][39][40] The
procedure involves five steps: polymer
dissolution, liquid-liquid or liquid-solid
phase separation, polymer gelation,
extraction of solvent from the gel with
water, and freezing and freeze-drying
under vacuum.[1][6] Thermal-induced
phase separation method is widely used
to generate scaffolds for tissue
regeneration.[40]

The homogenous polymer solution in the

first step is thermodynamically unstable
and tends to separate into polymer-rich
and polymer-lean phases under
appropriate temperature. Eventually after
solvent removal, the polymer-rich phase
solidifies to form the matrix and the
polymer-lean phase develops into
pores.[39] Next, two types of phase
separation can be carried out on the
polymer solution depending on the
desired pattern. Liquid-liquid separation
is usually used to form bicontinuous
phase structures while solid-liquid phase
separation is used to form crystal
structures. The gelation step plays a
crucial role in controlling the porous
morphology of the nanofibrous matrices.
Gelation is influenced by temperature,
polymer concentration, and solvent
properties.[39][40] Temperature regulates
the structure of the fiber network: low
gelation temperature results in formation
of nanoscale fiber networks while high
gelation temperature leads to the
formation of a platelet-like structure.[1]
Polymer concentration affects fiber
properties: an increase in polymer
concentration decreases porosity and
increases mechanical properties such as
tensile strength. Solvent properties
influence morphology of the scaffolds.
After gelation, gel is placed in distilled
water for solvent exchange. Afterwards,
the gel is removed from the water and
goes through freezing and freeze-drying.
It is then stored in a desiccator until
characterization.

Drawing

The drawing method makes long single

strands of nanofibers one at a time. The
pulling process is accompanied by
solidification that converts the dissolved
spinning material into a solid fiber.[37][41]
A cooling step is necessary in the case of
melt spinning and evaporation of solvent
in the case of dry spinning. A limitation,
however, is that only a viscoelastic
material that can undergo extensive
deformations while possessing sufficient
cohesion to survive the stresses
developed during pulling can be made
into nanofibers through this
process.[37][42]

Template synthesis

The template synthesis method uses a

nanoporous membrane template
composed of cylindrical pores of uniform
diameter to make fibrils (solid nanofiber)
and tubules (hollow nanofiber).[43][44]
This method can be used to prepare
fibrils and tubules of many types of
materials, including metals,
semiconductors and electronically
conductive polymers.[43][44] The uniform
pores allow for control of the dimensions
of the fibers so nanofibers with very
small diameters can be produced
through this method. However, a
drawback of this method is that it cannot
make continuous nanofibers one at a
time.

Self-assembly

The self-assembly technique is used to

generate peptide nanofibers and peptide
amphiphiles. The method was inspired
by the natural folding process of amino
acid residues to form proteins with
unique three-dimensional structures.[45]
The self-assembly process of peptide
nanofibers involves various driving forces
such as hydrophobic interactions,
electrostatic forces, hydrogen bonding
and van der Waals forces and is
influenced by external conditions such as
ionic strength and pH.[46]

Polymer materials

Collagen fibers in a cross-sectional area of dense

connective tissue.

Due to their high porosity and large

surface area-to-volume ratio, nanofibers
are widely used to construct scaffolds
for biological applications.[1][2] Major
examples of natural polymers used in
scaffold production are collagen,
cellulose, silk fibroin, keratin, gelatin and
polysaccharides such as chitosan and
alginate. Collagen is a natural
extracellular component of many
connective tissues. Its fibrillary structure,
which varies in diameter from 50-500 nm,
is important for cell recognition,
attachment, proliferation and
differentiation.[2] Using type I collagen
nanofibers produced via electrospinning,
Shih et al. found that the engineered
collagen scaffold showed an increase in
cell adhesion and decrease in cell
migration with increasing fiber
diameter.[47] Using silk scaffolds as a
guide for growth for bone tissue
regeneration, Kim et al. observed
complete bone union after 8 weeks and
complete healing of defects after 12
weeks whereas the control in which the
bone did not have the scaffold displayed
limited mending of defects in the same
time period.[48] Similarly, keratin, gelatin,
chitosan and alginate demonstrate
excellent biocompatibility and bioactivity
in scaffolds.[2]

However, cellular recognition of natural

polymers can easily initiate an immune
response.[2][38] Consequently, synthetic
polymers such as poly(lactic acid) (PLA),
polycaprolactone (PCL), polyurethane
(PU), poly(lactic-co-glycolic acid) (PLGA),
poly(L-lactide) (PLLA), and poly(ethylene-
co-vinylacetate) (PEVA) have been
developed as alternatives for integration
into scaffolds. Being biodegradable and
biocompatible, these synthetic polymers
can be used to form matrices with a fiber
diameter within the nanometer range.
Out of these synthetic polymers, PCL has
generated considerable enthusiasm
among researchers.[49] PCL is a type of
biodegradable polyester that can be
prepared via ring-opening polymerization
of ε-caprolactone using catalysts. It
shows low toxicity, low cost and slow
degradation. PCL can be combined with
other materials such as gelatin, collagen,
chitosan, and calcium phosphate to
improve the differentiation and
proliferation capacity (2, 17).[2][49] PLLA is
another popular synthetic polymer. PLLA
is well known for its superior mechanical
properties, biodegradability and
biocompatibility. It shows efficient cell
migration ability due to its high spatial
interconnectivity, high porosity and
controlled alignment.[50] A blend of PLLA
and PLGA scaffold matrix has shown
proper biomimetic structure, good
mechanical strength and favorable
bioactivity.

Applications
Tissue engineering

Bone matrix composed of collagen fibrils. Nanofiber

scaffolds are able to mimic such structure.

In tissue engineering, a highly porous

artificial extracellular matrix is needed to
support and guide cell growth and tissue
regeneration.[1][2][51][52] Natural and
synthetic biodegradable polymers have
been used to create such scaffolds.[1][2]
Simon, in a 1988 NIH SBIR grant report,
showed that electrospinning could be
used to produced nano- and submicron-
scale polystyrene and polycarbonate
fibrous mats specifically intended for use
as in vitro cell substrates. This early use
of electrospun fibrous lattices for cell
culture and tissue engineering showed
that Human Foreskin Fibroblasts (HFF),
transformed Human Carcinoma (HEp-2),
and Mink Lung Epithelium (MLE) would
adhere to and proliferate upon the
fibers.[53]

Nanofiber scaffolds are used in bone

tissue engineering to mimic the natural
extracellular matrix of the bones.[6][39]
The bone tissue is arranged either in a
compact or trabecular pattern and
composed of organized structures that
vary in length from the centimeter range
all the way to the nanometer scale.
Nonmineralized organic component (i.e.
type 1 collagen), mineralized inorganic
component (i.e. hydroxyapatite), and
many other noncollagenous matrix
proteins (i.e. glycoproteins and
proteoglycans) make up the
nanocomposite structure of the bone
ECM.[51] The organic collagen fibers and
the inorganic mineral salts provide
flexibility and toughness, respectively, to
ECM.
Although the bone is a dynamic tissue
that can self-heal upon minor injuries, it
cannot regenerate after experiencing
large defects such as bone tumor
resections and severe nonunion fractures
because it lacks the appropriate
template.[1][6][39] Currently, the standard
treatment is autografting which involves
obtaining the donor bone from a non-
significant and easily accessible site (i.e.
iliac crest) in the patient own body and
transplanting it into the defective site.
Transplantation of autologous bone has
the best clinical outcome because it
integrates reliably with the host bone and
can avoid complications with the
immune system.[54] But its use is limited
by its short supply and donor site
morbidity associated with the harvest
procedure.[51] Furthermore, autografted
bones are avascular and hence are
dependent on diffusion for nutrients,
which affects their viability in the host.[54]
The grafts can also be resorbed before
osteogenesis is complete due to high
remodeling rates in the body.[51][54]
Another strategy for treating severe bone
damage is allografting which transplants
bones harvested from a human cadaver.
However, allografts introduce the risk of
disease and infection in the host.[54]

Bone tissue engineering presents a

versatile response to treat bone injuries
and deformations. Nanofibers produced
via electrospinning mimics the
architecture and characteristics of
natural extracellular matrix particularly
well. These scaffolds can be used to
deliver bioactive agents that promote
tissue regeneration.[2] These bioactive
materials should ideally be
osteoinductive, osteoconductive, and
osseointegratable.[51] Bone substitute
materials intended to replace autologous
or allogeneic bone consist of bioactive
ceramics, bioactive glasses, and
biological and synthetic polymers. The
basis of bone tissue engineering is that
the materials will be resorbed and
replaced over time by the body’s own
newly regenerated biological tissue.[52]

Tissue engineering is not only limited to

the bone: a large amount of research is
devoted to cartilage,[55] ligament,[56]
skeletal muscle,[57] skin,[58] blood
vessel,[59] and neural tissue
engineering[60] as well.

Drug delivery

Successful delivery of therapeutics to the

intended target largely depends on the
choice of the drug carrier. The criteria for
an ideal drug carrier include maximum
effect upon delivery of the drug to the
target organ, evasion of the immune
system of the body in the process of
reaching the organ, retention of the
therapeutic molecules from preparatory
stages to the final delivery of the drug,
and proper release of the drug for
exertion of the intended therapeutic
effect.[7]

Nanofibers have grabbed the attention of

researchers as a favorable carrier
candidate.[8][9][61] Natural polymers such
as gelatin and alginate make for good
fabrication biomaterials for carrier
nanofibers because of their
biocompatibility and biodegradability that
result in no harm to the tissue of the host
and no toxic accumulation in the human
body, respectively. Additionally, the
physical properties of the nanofibers are
well suited for drug delivery
system.[1][2][5] Due to their cylindrical
morphology, they possess a high surface
area-to-volume ratio. As a result, the
fibers possess high drug-loading
capacity and can release therapeutic
molecules over a large surface area in
the medium.[38][7] Whereas surface area
to volume ratio can only be controlled by
adjusting the radius for spherical
vesicles, nanofibers have more degrees
of freedom in controlling the ratio by
varying both the length and the cross-
sectional radius. This adjustability is
important for their application in drug
delivery system in which the functional
parameters need to be precisely
controlled.[7]

Drugs and biopolymers can be loaded onto

nanofibers via simple adsorption, nanoparticles
adsorption, and multilayer assembly.

Antibiotics and anticancer drugs have

been successfully encapsulated in
electrospun nanofibers by adding the
drug into the polymer solution prior to
electrospinning.[62][63] Ignatova et al.
showed that various antibiotics such as
tetracycline hydrochloride, ciprofloxacin
and levofloxacin can be incorporated into
the synthetic polymer solution that can
be electrospun to produce fibers that can
be delivered to the site of interest.[64]
Drugs and other biopolymers such as
DNA can be loaded onto the surfaces of
nanofibers via simple adsorption,
nanoparticles adsorption, and multilayer
assembly. Surface-loaded nanofiber
scaffolds are useful as adhesion barriers
between internal organs and tissues
post-surgery.[65][66] Adhesion occurs
during the healing process and can bring
on complications such as chronic pain
and reoperation failure.[64][65][66]
Nanofibers can separate the surgery-
operated site from nearby tissues and
organs while simultaneously deliver
therapeutics such as antibiotics that are
physically adsorbed onto their surfaces.
Drugs can also be constructed in the
form of nanoparticles and attached to
the surface of nanofibers, allowing for
loading of high concentration of the
drugs in a given nanofiber. Rujitanaroj et
al. showed that nanofibers functionalized
with silver nanoparticles can be used as
effective antibiotics against bacteria
such as E. coli, Pseudomonas aeruginosa,
Staphylococcus aureus, and methicillin-
resistant Staphylococcus aureus found in
burn wounds.[67] Finally, charged
biopolymers such as DNA can be
incorporated into the multilayer assembly
of nanofibers.[68] Such modification can
provide diverse drug releasing surface
profiles of nanofibers for different
medical contexts.

Cancer diagnosis

Although pathologic examination is the

current standard method for molecular
characterization in testing for the
presence of biomarkers in tumors, these
single-sample analyses fail to account
for the diverse genomic nature of
tumors.[10] Considering the invasive
nature, psychological stress, and the
financial burden resulting from repeated
tumor biopsies in patients, biomarkers
that could be judged through minimally
invasive procedures, such as blood
draws, constitute an opportunity for
progression in precision medicine.

Liquid biopsy is an option that is

becoming increasingly popular as an
alternative to solid tumor biopsy.[10][11]
This is simply a blood draw that contains
circulating tumor cells (CTCs) which are
shed into the bloodstream from solid
tumors. Patients with metastatic cancer
are more likely to have detectable CTCs
in the bloodstream but CTCs also exist in
patients with localized diseases. It has
been found that the number of CTCs
present in the bloodstream of patients
with metastatic prostate and colorectal
cancer is prognostic of the overall
survival of tumors.[12][69] CTCs also have
been demonstrated to inform prognosis
in earlier stages of the disease.[70]

CTC capture and release mechanism of third

generation Thermoresponsive Chip.

Recently, Ke et al. developed a

NanoVelcro chip that captures the CTCs
from the blood samples.[11] When blood
is passed through the chip, the
nanofibers coated with protein
antibodies bind to the proteins expressed
on the surface of cancer cells and act
like Velcro to trap CTCs for analysis. The
NanoVelcro CTC assays underwent three
generations of development. The first
generation NanoVelcro Chip was created
for CTC enumeration for cancer
prognosis, staging, and dynamic
monitoring.[71] The second generation
NanoVelcro-LCM was developed for
single-cell CTC isolation.[72][73] The
individually isolated CTCs can be
subjected to single-CTC genotyping. The
third generation Thermoresponsive Chip
allowed for CTC purification.[11][74] The
nanofiber polymer brushes undergo
temperature-dependent conformational
changes to capture and release CTCs.

Lithium-air battery

Among many advanced electrochemical

energy storage devices, rechargeable
lithium-air batteries are of particular
interest due to their considerable energy
storing capacities and high power
densities.[13][14] As the battery is being
used, lithium ions combine with oxygen
from the air to form particles of lithium
oxides, which attach to carbon fibers on
the electrode. During recharging, the
lithium oxides separate again into lithium
and oxygen which is released back into
the atmosphere. This conversion
sequence is highly inefficient because
there is significant voltage difference of
more than 1.2 volts between the output
voltage and the charging voltage of the
battery meaning that approximately 30%
of the electrical energy is lost as heat
when the battery is charging.[13] Also the
large volume changes resulting from
continuous conversion of oxygen
between its gaseous and solid state puts
stress on the electrode and limits its
lifetime.

S h ti f lithi i b tt F th fib
Schematic of a lithium-air battery. For the nanofiber-
based lithium-air battery, the cathode would be
made up of carbon nanofibers.

The performance of these batteries

depends on the characteristics of the
material that makes up the cathode.
Carbon materials have been widely used
as cathodes because of their excellent
electrical conductivities, large surface
areas, and chemical stability.[15][75]
Especially relevant for lithium-air
batteries, carbon materials act as
substrates for supporting metal oxides.
Binder-free electrospun carbon
nanofibers are particularly good potential
candidates to be used in electrodes in
lithium-oxygen batteries because they
have no binders, have open macroporous
structures, have carbons that support
and catalyze the oxygen reduction
reactions, and have versatility.[76]

Zhu et al. developed a novel cathode that

can store lithium and oxygen in the
electrode they named nanolithia which is
a matrix of carbon nanofibers
periodically embedded with cobalt
oxide.[77] These cobalt oxides provide
stability to the normally unstable
superoxide-containing nanolithia. In this
design, oxygen is stored as LiO2 and
does not convert between gaseous and
solid forms during charging and
discharging. When the battery is
discharging, lithium ions in nanolithia and
react with superoxide oxygen the matrix
to form Li2O2, and Li2O. The oxygen
remains in its solid state as it transitions
among these forms. The chemical
reactions of these transitions provide
electrical energy. During charging, the
transitions occur in reverse.

Optical sensors

Polymer optical fibers have generated

increasing interest in recent years.[16][17]
Because of low cost, ease of handling,
long wavelength transparency, great
flexibility, and biocompatibility, polymer
optical fibers show great potential for
short-distance networking, optical
sensing and power delivery.[18][78]

Electrospun nanofibers are particularly

well-suitable for optical sensors because
sensor sensitivity increases with
increasing surface area per unit mass.
Optical sensing works by detecting ions
and molecules of interest via
fluorescence quenching mechanism.
Wang et al. successfully developed
nanofibrous thin film optical sensors for
metal ion (Fe3+ and Hg2+) and 2,4-
dinitrotoluene (DNT) detection using the
electrospinning technique.[16]

Quantum dots show useful optical and

electrical properties, including high
optical gain and photochemical stability.
A variety of quantum dots have been
successfully incorporated into polymer
nanofibers.[79] Meng et al. showed that
quantum dot-doped polymer nanofiber
sensor for humidity detection shows fast
response, high sensitivity, and long-term
stability while requiring low power
consumption.[80]

Kelly et al. developed a sensor that warns

first responders when the carbon filters
in their respirators have become
saturated with toxic fume particles.[19]
The respirators typically contain
activated charcoal that traps airborne
toxins. As the filters become saturated,
chemicals begin to pass through and
render the respirators useless. In order to
easily determine when the filter is spent,
Kelly and his team developed a mask
equipped with a sensor composed of
carbon nanofibers assembled into
repeating structures called photonic
crystals that reflect specific wavelengths
of light. The sensors exhibit an iridescent
color that changes when the fibers
absorb toxins.

Air filtration

Paints and protective coatings on furniture contain

Paints and protective coatings on furniture contain
volatile organic compounds such as toluene and
formaldehyde.

Electrospun nanofibers are useful for

removing volatile organic compounds
(VOC) from the atmopshere. Scholten et
al. showed that adsorption and
desorption of VOC by electrospun
nanofibrous membrane were faster than
the rates of conventional activated
carbon.[20]

Airborne contamination in the personnel

cabins of mining equipment is of
concern to the mining workers, mining
companies, and government agencies
such as the Mine Safety and Health
Administration (MSHA). Recent work
with mining equipment manufacturers
and the MSHA has shown that nanofiber
filter media can reduce cabin dust
concentration to a greater extent
compared to standard cellulose filter
media.[21]

Oil-water separation

Nanofibre has the capabilities in oil–

water separation, most particularly in
sorption process when the material in
use has the oleophilic and hydrophobic
surfaces. These characteristic enable the
nanofiber to be used as a tool to combat
either oily waste- water from domestic
household and industrial activities, or oily
seawater due to the oil run down to the
ocean from oil transportation activities
and oil tank cleaning on a vessel.[31]

See also
Subwavelength-diameter optical fiber
Nanofiber seeding
Polyaniline nanofibers

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