The History of Electrospinning 1683523794

REVIEW
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The History of Electrospinning: Past, Present, and Future

Developments
Antonios Keirouz,* Zhe Wang, Vundrala Sumedha Reddy, Zsombor Kristóf Nagy,
Panna Vass, Matej Buzgo, Seeram Ramakrishna, and Norbert Radacsi*
nanofibers (NFs), and the ease of manip-

Electrospinning has rapidly progressed over the past few decades as an easy ulating the composition and properties
and versatile way to fabricate fibers with diameters ranging from micrometers of the fibers formed, electrospinning
to tens of nanometers that present unique and intricate morphologies. This has been at the cutting edge in the re-
has led to the conception of new technologies and diverse methods that search and industrialization of advanced
fiber-based materials.[1,2] Compared
exploit the basic electrohydrodynamic phenomena of the electrospinning to other methods of fabricating fibers
process, which has in turn led to the invention of novel apparatuses that have within the sub-micrometer/nanoscale,
reshaped the field. Research on revamping conventional electrospinning has electrospinning is regarded as a scalable,
principally focused on achieving three key objectives: upscaling the process cost-effective, and reasonably automated
while retaining consistent morphological traits, developing 3D nanofibrous route of low-labor manufacturing that
has continuously gained ground over
macrostructures, and formulating novel fiber configurations. This review
the past two decades.[3] Electrospun
introduces an extensive group of diverse electrospinning techniques and fibers have been widely applied in many
presents a comperative study based on the apparatus type and output. Then, fields: tissue engineering,[4–7] drug
each process’s advantages and limitations are critically assessed to identify delivery,[4] sensing,[5] filtration,[10,11]
the bona fide practicability and relevance of each technological breakthrough. wound dressings,[6,7] self-cleaning
[8,9]
Finally, the outlook on future developments of advanced electrospinning surfaces, biotechnology,[10] envi-
ronmental engineering,[11] and green
technologies is outlined, with an emphasis on upscaling, translational chemistry[12–14] are a few of the many
research, sustainable manufacturing and prospective solutions to current areas in which electrospinning has been
shortcomings. explored, among others.
Although conventional electrospin-
ning is a reasonably flexible and straight-
forward method that can effortlessly
1. Introduction produce peculiar fiber morphologies from a range of
polymer-solvent systems and complex dopants, includ-
Due to their attractive properties associated with an immense ing nanomaterials,[15,16] graphene,[17,18] and pharmaceutical
length-to-diameter ratio, the capability of producing smooth compounds,[4] it is unanimously accepted by the scientific
A. Keirouz, Z. Wang, N. Radacsi A. Keirouz

School of Engineering Centre for Bioengineering and Biomedical Technologies (CBio)
Institute for Materials and Processes Department of Chemical Engineering
The University of Edinburgh University of Bath
King’s Buildings, Edinburgh EH9 3FB, UK Bath BA2 7AY, UK
E-mail: keirouz.antonios@gmail.com; n.radacsi@ed.ac.uk V. S. Reddy, S. Ramakrishna
A. Keirouz Centre for Nanotechnology and Sustainability
Empa Department of Mechanical Engineering
Swiss Federal Laboratories for Materials Science and Technology National University of Singapore
Biomimetic Membranes and Textiles Singapore 119260, Singapore
St. Gallen CH-9014, Switzerland Z. K. Nagy, P. Vass
Department of Organic Chemistry and Technology
The ORCID identification number(s) for the author(s) of this article Budapest University of Technology and Economics (BME)
can be found under https://doi.org/10.1002/admt.202201723 Műegyetem rakpart 3, Budapest H-1111, Hungary
© 2023 The Authors. Advanced Materials Technologies published by M. Buzgo
Wiley-VCH GmbH. This is an open access article under the terms of the Biofabics
Creative Commons Attribution License, which permits use, distribution R. Alfredo Allen 455, Porto 4200-135, Portugal
and reproduction in any medium, provided the original work is properly
cited.
DOI: 10.1002/admt.202201723
Adv. Mater. Technol. 2023, 2201723 2201723 (1 of 34) © 2023 The Authors. Advanced Materials Technologies published by Wiley-VCH GmbH
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community that exceeding the associated fiber output limitations Formhals in 1934.[30] Between 1964 and 1969, Geoffrey Taylor, ap-
is challenging.[19] This is because conventional electrospinning pertaining to Zeleny’s work, mathematically demonstrated that
produces a single jet stream deriving from a single Taylor cone the critical half-angle of the meniscus nears 49.3° at the furthest
during fabrication, thus exhibiting a low yield of ≈0.01–0.3 g point before the disintegration event, illustrating why a polymer
h−1 .[20] To address this limitation, researchers have devoted solution or melt extruded through a capillary will reshape from a
considerable effort to resolving this challenge. Notably, between spherical to a conical configuration in a strong electric field.[31,32]
2004 and 2005, Ding et al.[21] and Theron et al.[22] found a simple This gave rise to the concept of the "Taylor cone" formation. How-
way to significantly increase the fiber output by using multiple ever, no significant electrospinning developments were reported
jet streams instead of a single nozzle. However, this approach in the literature in the following two decades. This loss of atten-
proved to be time-consuming and involved a tedious spinneret tion from academia and industry coincides with the lack of accu-
cleaning cycle to avoid interactions between jets.[3] Later, Do- rate methods to observe the morphology and measure the diam-
sunmu et al. designed a new type of electrospinning setup using eter of fibers down to the sub-micrometer scale.
a multi-hole prous cylindrical tube to further increase the output It was not until the early 1990s, due to the increasing inter-
of the process, reaching up to 1 g h-1 .[23] However, the porous est in nanotechnology, that the study of electrospinning technol-
cylinder spinneret capable of vertically orienting its axis could ogy started to gain popularity.[33] The modern era of electrospin-
only deposit fibers in a 360° cylindrical collector surrounding ning began with work conducted by Jayesh Doshi and Darrell
the spinneret, resulting in inconcistent fibrous membranes due Reneker,[34] who reported that the diameter of the fibers is inverse
to secondary electrical effects and the ease of spinneret clogging. proportional to the distance from the needle tip to the collector.
These issues were resolved by a method developed by Yarin From 1999 to 2001, Reneker and Gregory Rutledge worked to bet-
and Zussman in 2004[19] that paved the way for all the high- ter understand the parameters influencing the electrospinning
throughput electrospinning technologies that followed. This process,[35,36] owing to the advancement of scanning electron mi-
method involved the production of free-surface NFs through a croscopy (SEM) that enabled fibers within the nanometer scale to
two-layer system. By placing a layer of polymer solution under- be observed in detail. These advancements commended the ca-
neath a magnetic liquid that overlapped a permanent magnet pabilities of electrospinning to the scientific community for the
against a vertically placed oppositely charged magnet by apply- first time.
ing high DC voltage, for the first time, jets formed without a As depicted in Figure 1, electrospinning has gained signifi-
needle-based spinneret. A year later, Jiri and co-workers patented cant attention since the turn of the century, with a consistent
a process where a rotating charged electrode, immersed within exponential increase in the number of published works in the
a polymer solution, placed at a close distance to a counter elec- field. Studies surrounding the working electrospinning parame-
trode in a bottom-up position, could be used to fabricate NFs at ters and understanding how different polymers can be processed
an increased production rate with the assistance of an airstream into fibers flourished. This was followed by research groups de-
to increase the auxiliary drying efficiency of the system.[24] Grad- veloping novel electrospinning apparatuses, including co-axial,
ually, more needleless electrospinning methods were reported, tri-axial, centrifugal, corona, bubble, rotary metals (cylinder, disk,
further improving the productivity and quality of the fibers with ball), high-speed, and 3D electrospinning (Table 1), which are
the primary purpose of achieving industrial-scale NF production. expounded in this review. These advanced techniques have ex-
This comprehensive review critically discusses the history and panded the range of materials that can be used to fabricate fibers
evolution of electrospinning technology. A detailed introduction and the gamut of obtainable structures. The main principles
to the most used electrospinning techniques is succeeded by a behind developing these apparatuses has been to improve the
comparative study focusing on the advantages and disadvantages fiber output and the fibers’ macro and microarchitecture, further
of each method. Thereafter, the limitations of the different tech- widening the reach of electrospun materials.
niques are discussed, followed by an outlook on the future of ad-
vanced electrospinning technologies. 3. Background and Classification
2. Brief History 3.1. Principles and Process Parameters
A lengthy chronology of inventions and innovations accompanies Among the processing techniques, including thermal-induced
the history and progress of electrospinning. Electrospinning is phase separation, drawing, template synthesis, and self-
the descendant of electrospraying, a conceptually similar tech- assembly, electrospinning is of considerable significance as
nology that employs electric forces to disperse a liquid or fine a rapidly evolving fiber preparation method.[52] This highly
aerosols out of a polymer solution, first carried out in 1747 by versatile method is used to process solutions, suspensions, or
Abbé Nollet[25] and first patented by John Cooley[26] and William melts into continuous fibers of nano/microscale diameters[53]
Morton[27] in the early 1900s. When electrospinning, a fluid with- and is the only method capable of mass-producing continuous
drawn through the spinneret is electrically charged, acquiring fibers at this range.[54]
a nearly conical shape from the apex of which a jet arises.[28] Electrospinning is one of the most conventional methods used
In 1914, John Zeleny first demonstrated that the jet ejection at for continuous fiber preparation today and is based on the prin-
the tip of the metal capillary presents a liquid drop surface ten- ciple that electrostatic forces can be used to form and expand
sion held at the edge that disintegrates onto a spray as the volt- fibers out of a polymer solution.[55] As expounded in the pre-
age increases.[29] Later, the earliest method of producing nanofi- vious section, the principle of this process was first described
brous materials from polymer solutions was patented by Anton in the 1930s in a patent entitled "Process and Apparatus for
Figure 1. Progress in electrospinning research based on publication output over the years. Data obtained from Scopus (Elsevier) based on the searching
command "TITLE-ABS-KEY electrospinning OR electrospun OR electrospin* AND LIMIT-TO ( DOCTYPE , "ar" )".
Table 1. Milestones in the development of electrospinning methods. uses electrostatic forces to produce and expand fibers from poly-
mer solutions or melts with diameters ranging from a few tens
Electrospinning methods Year Inventor References of nanometers to micrometers.[55] During electrospinning, high
Mono-axial 1902 Cooley and Morton [26,27]
voltage is applied to charge a liquid solution or melt by placing it
between two conductors that endure the electromagnetic charge
Co-axial 2003 Sun et al. [37]
of opposite polarities, stretching the polymer to form fibers.[57]
Multijet 2004 Ding et al. [21]
A standard laboratory-scale setup consists of four main compo-
Magnetic fluid 2004 Yarin et al. [19]
nents: a high-voltage DC (or AC) power supply, a syringe pump,
Roller 2005 Jirsak et al. [24] a nozzle (usually a metallic capillary), and a collector (which can
Centrifugal 2006 Andrady et al. [38] be a metallic foil, plate, or disc). The electrostatic force produced
Porous tube 2006 Dosunmu et al. [23] by the high-voltage supply is applied to the polymer solution or
Bubble 2008 Liu et al. [39] melt, which is dispensed through the fine needle orifice at a con-
Tri-axial 2009 Kalra et al. [40] trolled rate. When electrospinning, the precursor solution ex-
Conical wire coil 2009 Wang et al. [41] truded from the spinneret orifice forms a small droplet that is
Ball 2009 Miloh et al. [42] subject to an accumulated charge in the presence of an electric
Disk 2009 Niu et al. [43]
field.[58] The electric discharged of the polymer droplet, induces
a conically-shaped geometry referred to as the Taylor cone.[59,60]
Wet (3D) 2009 Yokoyama et al. [44]
Increasing the strength of the electric field causes an increased
Cone 2010 Lu et al. [3]
accumulation of charges at the surface of the polymer bud. Af-
Spiral coil 2012 Wang et al. [45]
ter this, the repulsive electric forces overcome the surface ten-
Corona 2012 Molnár et al. [46] sion of the polymer solution or melt, leading to vigorous whip-
Stepped pyramid 2013 Jiang et al. [47] ping and splitting motions due to the bending instabilities gen-
Beaded chain 2014 Liu et al. [48] erated, causing the fiber to elongate through the application of
High-speed 2015 Nagy et al. [49] mechanical force.[61] At this point, the geometry of the formed
Cold-plate (3D) 2015 Sheikh et al. [50] asymmetrically electrospun (as-spun) fibers is directed by the
Three-dimensional (3D) 2018 Vong et al. [51] electrostatic repulsion, colloid stability, the incoming surface ra-
tio, and gravity.[55,57] The solidification of the liquid solution oc-
curs by establishing a zone that thrusts the charged molecules, al-
lowing for continuous solvent evaporation, stretching the drawn
Preparing Artificial Threads" by Anton Formhals, considered polymer threads as they advance toward the grounded or op-
the father of electrospinning.[56] However, considerable empha- positely charged collector.[55] This transition between the liquid
sis was not given to the process until the 1990s in works led by and solid phase is due to the Ohmic current primarily being
Reneker and Rutledge, who described the process.[34] transited to convective flow, thus increasing its acceleration.[62]
The electrospinning process is related to an electrohydrody- Figure 2 illustrates the basic concept behind the electrospinning
namic problem. It is a simple and cost-effective method that process.
Figure 2. Fundamentals of electrospinning. a) Schematic representation of the electrospinning concept (created with Biorender); b) high-speed photo-
graph outlining the Taylor cone formation, depicting the linear segment of the polymer jet, followed by the whipping jet region, modified from refs. [63]
and [64]; c) the prototypical instantaneous position of the jet path succeeding through the three sequential bending instabilities, modified from ref. [58],
Copyrights: (a) created with BioRender; (b) Adapted (right segment) with permission.[63] Copyright 2013, AIP Publishing; (b) Adapted (left segment)
with permission.[64] Copyright 2007, Elsevier; (c) Adapted with permission.[58] Copyright 2019, American Chemical Society.
The formed electrospun mats exhibit a web-like fibrous struc- The parameters influencing the electrospinning process[77]
ture due to the considerable extent of plastic deformation caused can be classified based on solution and solvent, operating, and
by the high charge density of the jet and the unstable whip- ambient conditions (Figure 4). Solution parameters refer to poly-
ping motion.[65] This phenomenon is known as bending insta- mer concentration and polymer molecular weight, solvent volatil-
bility, and it leads to randomly oriented and nonaligned fibrous ity, solution viscosity, surface tension, and solution conductivity,
mats.[66] among others. Concerning the electrospinning parameters, the
NFs carry a range of novel physical and chemical proper- electric field strength, electrostatic potential, flow rate, and dis-
ties that are not present in their corresponding macroscales, re- tance between the spinneret and the collector must be appropri-
sulting in many characteristics shared among materials at the ately adjusted in conjunction with the polymer solution proper-
nanoscale.[67] Due to high specific surface area, a large surface- ties. Finally, ambient parameters refer to the chamber and solu-
to-volume ratio, and an extensive fiber length-to-diameter as- tion temperature, humidity, and type of atmosphere, among oth-
pect ratio, properties such as peculiar quantum effects, electri- ers.
cal conductivity, redox potential, and the formation of crystal In general, by prolonging the fiber elongation or flight time
and magnetic structures increase their reaction rates per given during the electrospinning process, finer fibers can be produced,
mass.[65] Moreover, those properties allow the construction of which can be achieved by increasing the distance between the
highly porous constructs with adjustable pore size and wide sur- collector and the spinneret. Moreover, the evaporation rate of the
faces that allow chemical functionalization.[65] solvent can be increased by using low-volatility solvents and rais-
Through the continuous research and evolvement of these ba- ing the chamber temperature. However, it must be noted that in-
sic principles and the manipulation of the conventional electro- creasing the working distance beyond the critical threshold (the
spinning apparatus, unique morphologies and structures have point at which the stability of the Taylor cone is impaired) re-
been successfully produced over the past two decades, as indi- sults in a significantly longer flight time, which can lead to inho-
cated in the examples presented in Figure 3. mogeneous fiber formation.[4] Insufficient solvent volatility and
Figure 3. Structural diversity of individual electrospun fiber morphologies: a) aligned; b) randomly oriented; c) core/shell;[68] d) hollow;[68] e) multi-
channel microtubes;[69] f) colloidal nanoparticle-decorated;[70] g) shish-kebab;[71] h) helical;[72] i) porous; j) necklace-like;[73] k) island-like;[74] l) beads-
in-fiber,[75] electrospun fibers. Copyrights: (c, d) Reproduced with permission.[68] Copyright 2004, American Chemical Society; (e) Reproduced with
permission.[69] Copyright 2007, American Chemical Society; (f) Reproduced with permission.[70] Copyright 2013, American Chemical Society; (g) Re-
produced with permission.[71] Copyright 2021, Royal Society of Chemistry; (h) Reproduced with permission.[72] Copyright 2012, American Chemical
Society; (i) Produced from author A.K. (j) Reproduced with permission.[73] Copyright 2008, Elsevier; (k) Reproduced with permission.[74] Copyright
2017, American Chemical Society; (l) Reproduced with permission.[75] Copyright 2020, Springer Nature.
low temperatures may lead to wet fiber fusion during deposition. the polymer solution from the molecular weight and its concen-
Therefore, the parameters that affect the electrospinning process tration. Within a solution, the root-mean-square distance of the
must be observed and monitored to determine the ideal operating segment of a molecular chain toward the center of its mass pro-
conditions that can yield optimized fiber characteristics tailored vides the average radius of gyration (Rg ).[76] If the concentration
to the specific requirements of each study. is too low (diluted solutions), the polymer chains do not overlap,
One of the most important parameters for obtaining an elec- with the viscoelasticity of the solution being governed by shorter
trospinnable solution is determining the chain entanglement of polymer chains. When the concentration of the polymer is in-
Figure 4. Schematic representation of the electrospinning processing parameters. Several criteria must function concurrently under optimal conditions
to attain a stable electrospinning process. These can be classified based on solution, operating, and ambient parameters. These conditions are further
responsible for the process’s production rate, physicochemical characteristics, and morphological properties.
creased, entanglement occurs as the polymeric chain begins to search surrounds the use of the conventional needle-based setup
overlap. with either a drum or a flat collector, significant research has
The critical concentration (Cc *) is generally accepted to be pro- focused on further manipulating the design of electrospinning
portional to the polymer’s molecular weight (Mw ) and the effec- devices based on the fundamental principles described in this
tive solvent volume section, to further advance the producibility and morphological
architecture of the fibers. For instance, co-axial and multi-axial
3Mw electrospinning apparatuses can produce fibers from highly di-
Cc∗ = (1)
4𝜋R3g NA verse polymer pairs, e.g., core–sheath, hollow, and nanoparticle-
decorated, while each one can maintain its separate material
where NA is the Avogadro constant.[77] If the polymer concentra- identity. A high fiber production rate can be achieved by increas-
tion is below the critical point (C < Cc *), inadequate chain entan- ing the surface area of the spinneret via technologies such as free-
glement can result in an unstable jet due to Rayleigh instabilities. surface and needleless electrospinning. 3D buildups can be con-
Therefore, for stable electrospinning, the polymer concentration veyed by incorporating 3D printing and electrospinning, whereas
needs to be higher than the critical point (C < Cc *).[78] In many ultrathin-aligned NFs are obtainable via centrifugal electrospin-
cases, the correlation between the Mw of a polymer solution and ning. Finally, portable electrospinning apparatuses have been de-
its corresponding Rg value is evident. Thus, in some instances, veloped for biomedical applications, where fibers can be directly
attempting to electrospin variant molecular weights of the same deposited into an open wound. As described in the following sec-
polymer can ultimately contribute to the procurement of the re- tions, advances in such apparatuses have managed to keep elec-
quired concentration (beyond Cc *) for effective and stable electrospinning on the frontline of research.
trospinning.
Selecting the ideal operating range of each electrospinning
condition can be challenging when designing an experiment, due
to the vast choice of polymers and the corresponding solvent sys- 3.2. Instrumentation
tems. Moreover, most parameters are interdependent, leading
to nonlinear causality, one of the significant challenges in the Despite the apparatus’s design and configuration, the electro-
electrospinning field. Understanding the parameters that influ- spinning process will always consist of three main components:
ence the electrospinnability of a polymer solution and the sub- a high-voltage power supply, a jet generator, and a collector.
sequent properties of the fibers formed has made it possible to When high-voltage power is applied to the spinneret, a strong
advance polymer chemistry and evolve the capabilities of the pro- electric field is created around a pendant droplet. This causes the
duced electrospun scaffolds. Though the majority of present re- droplet to overcome surface tension and, in the presence of suffi-
cient molecular cohesion, commences jetting. The jet is directed to interact with the polymer chains, taking into account the en-
by the movement of charged molecules from high to low voltage. ergy from the dispersion forces, the dipolar intermolecular force
The jet generator, commonly referred to as the spinneret, in- and hydrogen bonds.[77] Based on the selected solvent system, as
troduces the polymer solution into the electric field and facilitates described in the previous section, determining the critical con-
liquid distortion, Taylor cone formation, and jetting. The spin- centration can be advantageous. This can influence processing
neret is the principal component differing between needle-based stability by determining the necessary minimum solution con-
and needleless methods. In nozzle-based methods, the spinneret centration. Higher molecular weight polymers are more resistant
can be monopolar or consist of multineedle concentric arrange- to solvent dissolution and may require the application of heat be-
ments. In the case of needleless methods, the spinneret configu- low the polymer’s melting point, in order to avoid polymer degra-
ration can vary significantly in form, with structures such as wire, dation, while promoting solubilization.
corona, cylinder, ball, and bubble, among others. As a great number of parameters need to be met by a sol-
Finally, the collector, either grounded or charged oppositely to vent to induce stable jetting, it is a common practice to use
the spinneret, directs the travel path of the jet, allowing for the solvent-systems; mixtures consisting of two or more compat-
fibers to be deposited while discharging them at the collector’s ible solvents. In the realm of electrospinning, the most fre-
surface. Although the collector’s configuration does not play a quently utilized solvents are halogenated solvents (e.g., chloro-
significant role in the fiber production rate, it can influence fiber form, trifluoroethanol), tetrahydrofuran (THF), aprotic solvents
morphology and is responsible for the dimensions of the electro- (e.g., dimethylformamide [DMF], dimethylacetamide [DMAc],
spun membranes produced. Traditionally, a metallic plate is used dimethyl sulfoxide [DMSO]), and protic solvents (e.g., ethanol,
to produce randomly-oriented fiber mats, while a solid cylinder acetone, water).[14,81] Halogenated solvents remain at the fore-
at high revolutions per minute can introduce fiber alignment. front of lab-scale electrospinning research due to their high rates
Nonetheless, variant collectors have been reported in the liter- of hydrophobic polymer dissolution and low boiling point, which
ature, including roller, rotating wire drum, knife-edged, honey- is of special interest to polymers resistant to many standard or-
comb, and liquid bath, among others, capable of generating com- ganic solvents, such as fluoropolymers.[82]
plex fiber morphologies.[79,80] Industrial-size, commercial-scale As the electrospinning process moves towards upscaling
electrospinning units can provide continuous production lines technologies, larger amounts of solvents for fiber processing,
by depositing fibers in a supporting textile using a feed/take-up which has led to the investigation of green and sustainable sol-
dual cylinder system. This can significantly increase the output vents. This coincides with regulatory agencies, such as the Chem-
and dimensions of the produced materials to anywhere between ical Control Regulation in the European Union (REACH), set-
10 and 800 sq m h−1 and 0.01 and 2 g m−2 , respectively. For in- ting the rationale and strict limitations on the use of harmful sol-
stance, a thicker deposition will coincide with a smaller mem- vents (such as DMF, toluene, chloroform, and dichloromethane)
brane/fabric area; on this account, determining the solid content to prevent workplace exposure and environmental contamination
when measuring the output can be a better indicator. risks.[85] Along with the environmental impact and user safety,
the selection of green(er) solvents should also consider produc-
tion sustainability (e.g., emissions, energy efficient, whether it
3.3. Solvent Selection can be sourced from renewable sources), solvent recyclability,
and disposal.[86] An overview of several studies that have focused
Although it is feassible to procure electrospun fibers via solvent- on substituting harmful conventional solvents for green alterna-
free techniques, such as melt electrospinning and melt blowing, tive is provided in Table 3. As a relatively new area of interest in
the higher temperature required to melt the polymer during pro- response to society’s growing enviromental consciousness and
cessing can lead to thermal degradation, which limits the mate- focus on sustainability, green chemistry focused on electrospin-
rials that can be electrospun (e.g., small molecules, nanomate- ning is a critical research question that has yet to be fully ex-
rials, and bioactive compounds).[14] Moreover, melt spun fibers plored.
tend to have langer diameters, primarily due to the much higher
viscosity of polymer melts and poorer conductivity. Most of the
research conducted on electrospinning relies on solvent-based
methods, due to the greater flexibility, fewer limitations and the 3.4. Materials Selection
greater number of available technologies.
As described, in detail, in Table 2, at the end of the section, the The most prevalent research question that has propelled the ad-
polymer solution parameters are interdependent. For solution vancement of the field has been answering, “what can be elec-
electrospinning, a solvent must be able to solubilize the polymer trospun?”. This has given rise to a wide range of common and
homogeneously while sufficiently evaporating during jetting, in- intricate materials being successfully electrospun into fibers. Al-
ducing fiber solidification. The choice of solvent has a substantial though principally, electrospinning relies on polymeric materi-
impact on solution spinnability and the fiber morphology. Experi- als, ceramics, metals, and inorganic chemical compounds can
mentally, solvent selection is generally conducted by determining also be transformed into fibers in the presence of a carrier
the chemical structure and properties of the polymer, establish- polymer, which can be subsequently kept or removed through
ing a list of compatible solvents; based on their physical prop- postfabrication processing. In addition, small molecules can be
erties, and conducting short parametric studies focused on sol- electrospun by tuning their chemistry to attain sufficient poly-
ubilization and electrospinnability. Mathematically, the Hansen mer chain entanglement or by incorporating a readily electro-
solubility parameter can be used to estimate the solvent’s ability spinnable high molecular weight carrier polymer. As a broad clas-
Table 2. A detailed account of the solution, operating, and ambient parameters influencing the electrospinning process and fiber formation.
Parameters Influence on electrospinning
Solution parameters Molecular weight – The length of the polymer chains has a direct effect in facilitating or obstructing chain extensibility.
– Sufficient topological entanglements coupled with an appropriate solvent system are required.
– Generally, higher molecular mass polymers are associated with more uniform but thicker fibers.
While insufficient molecular mass will either hinder electrospinning or produce non-uniform fiber
mats.
Concentration – Composite blends generally produce larger fibers due to a denser polymer entanglement.
– Increasing the polymer concentration is associated with uniform and more elongated fibers with
no or fewer secondary morphologies (e.g., beads and spider webs) and a smaller fiber diameter
standard deviation.
– Low concentrations inhibit fiber formation due to inadequate surface tension, causing jet
fragmentation.
Viscosity – Viscosity increases as intermolecular interactions and/or molecular weight increase.
– Viscosity is dependent on the shear rate and temperature.
– Attaining appropriate viscosity during electrospinning can prevent polymer spraying (low) or the
formation of large-diameter fibers (high).
General note – Viscosity, molecular weight (Mw ), and concentration are intertwined. The average number of
entanglements per chain increases with Mw , whereas the entanglements per mass/volume
increase with concentration.[ 83]
Surface tension – Surface tension is responsible for instigating the electrohydrodynamic events of the
electrospinning process.
– Surface tension is associated with a liquid surface taking up the minimum surface area required
(the force required from a specific mass along a line of unit length).
– The electric field required to initiate electrospinning correlates to the surface tension, which, in
turn, will depend on the spinneret’s configuration.
– As the surface tension increases, a stronger electric field is needed to commence electrospinning.
This can sometimes be adjusted during electrospinning, e.g., beginning with higher voltage and
lowering it after a stable jet has formed.
– Surfactants can enhance electrospinnability by improving polymer spreading and/or increasing
the solution’s conductivity (especially for needleless spinnerets).
– Needleless electrospinning techniques require a higher voltage because of the higher surface
tension that must be devolved to instigate jet formation.
Conductivity and permittivity – Two electrostatic forces set in motion, Taylor cone formation and jetting; electrostatic repulsion
between the surface charges and a Coulombic force applied by the external electric field.[ 84 ]
– An appropriate solution conductivity increases the number of charges that can be carried out
while reducing the minimum voltage required for jet eruption.
– Although theoretically, the fiber diameter decreases with increased solution conductivity, by
promoting polymer stretching, in practice, a too-high conductivity will produce unstable jetting
due to electrical air discharges.
– Permittivity refers to the proportion of electric displacement toward the intensity of the electric
field. Reducing the solution’s permittivity can increase the electric field intensity.
– When insufficient, introducing small amounts of salt (e.g., NaCl, LiCl, tetraethylammonium
bromide [TEAB]) in the polymer solution can significantly increase the conductivity and
permittivity. This approach is commonly used in needleless electrospinning to increase fiber
output by increasing the number of formed Taylor cones.
Solvent parameters Solvent volatility and vapor – During electrospinning, fiber solidification relies on the solvent system’s evaporation rate, and
pressure thus the volatility of the selected solvent system can influence the morphology of the fibers.
– An adequate evaporation rate will allow the collection of dry membranes, while reducing the
degree of solvent entrapment.
– A too-volatile solution can induce morphological traits/defects (e.g., porous fibers in the presence
of a non-water-soluble polymer) or even hinder electrospinning.
– Vapor pressure can promote further solvent evaporation, generating noncylindrical secondary
morphologies, such as spider webs.
– A commonly used term in electrospinning, evaporation rate, will rely on a combination of
parameters being met alongside the solvent’s volatility, including relative humidity, working
distance, and spinneret configuration.
Dielectric constant – The dielectric constant refers to the solvent’s capability to retain the electrostatic repulsions
induced by the electric charge affecting the surface charge distribution.
– A higher dielectric constant will improve surface charge distribution and jet stability. For instance,
water presents a high dielectric constant that can weaken the electrostatic repulsions and is, thus,
commonly incorporated as part of solvent systems.
(Continued)
Table 2. (Continued).
Parameters Influence on electrospinning
Operating conditions General note – The operating condition requirements will differ greatly between needle-based and needleless
electrospinning technologies.
Applied voltage – As an electrohydrodynamic process, electrospinning relies on applying high voltage to a polymer
solution to initiate the process.
– A minimum threshold voltage influenced by the surface tension of the polymeric solution, referred
to as critical voltage, VK , must be surpassed for jet generation.
– Increasing the voltage above the required threshold generally reduces the jet’s "flight time,"
producing an unstable jet path with larger diameter fibers or secondary fiber morphologies.
– A voltage below the required threshold will, in most instances, spray the polymer solution onto the
collector or along the jet path.
– Needleless electrospinning technologies require a substantially higher Vk due to the greater
surface tension.
Solution feed (flow) rate – The flow rate, which is the amount of solution exposed to the high electric field at a given time, is
the main contributor affecting surface tension and the VK.
– The effect of the solution feed rate will be directly influenced by most of the parameters discussed
in this table. Increasing the flow rate will generally promote insufficient fiber stretching, which can
produce wet or thicker fibers with larger pores.
– Flow rate plays a key role in multi-axial needle-based electrospinning.
– Although, as a term, "flow rate" is not typically used in needleless electrospinning, the way that the
solution is introduced into the needleless spinneret (e.g., via cartilage, a solution bath, among
others) can positively or negatively affect the homogeneity of the produced fibrous membranes.
Working distance – Working distance refers to the distance between the spinneret and the collector, which defines the
jet path.
– Increasing the working distance can give more time for a less-volatile solvent to evaporate and for
the polymer to solidify. Expanding the jet path is also associated with thinner fibers and vice versa.
– Exceeding the critical distance can halt electrospinning or produce defective fibers due to
prolongated bending instabilities, affecting fiber branching
Collector geometry – The collector’s geometry can directly affect the micro and macromorphological properties of the
deposited fibers.
– A collector can provide alignment (e.g., a rotating mandrel), orientation (e.g., a cylindrical
collector surrounding a rotating spinneret), facile patterning (e.g., honeycomb mesh), and mass
production (e.g., supporting textile dual cylinder system).
Spinneret design – The spinneret type is the cardinal difference between needle-based and needleless electrospinning
and the principal focus of this review.
– The spinneret configuration will affect the output of each technology, the complexity and
architecture of the developed fibers (e.g., co-axial), and even the properties of the developed
constructs (e.g., 3D macrostructures or alignment due to a rotating spinneret).
Ambient conditions Temperature – The chamber temperature during electrospinning will affect the solution viscosity and surface
tension, the solvent’s evaporation rate, and the jet solidification rate.
– Depending on the polymer and solvent-system properties, the working temperature can positively
and negatively affect the process.
Relative humidity – High relative humidity can induce non-uniformity, and in the case of hygroscopic polymers,
unique fiber configurations (such as porous, dimpled, or pitted fibers) when other solution
parameters are sufficiently met.
– High humidity can also hinder electrospinning by affecting the total charge distribution and
reducing the surface charge density.
– Due to rapid solvent evaporation, very low humidity can reduce the flying jet path, producing
thicker fibers.
sification, these can be divided into three principal groups: or- rence, an extensive number of natural, synthetic, and semisyn-
ganic polymers, small molecules, and composite materials. thetic polymers have been manipulated into electrospun fibers.
Polymers of all forms; homopolymers, copolymers, and blends
can produce stable electrospinning solutions. Unlike copolymers
3.4.1. Organic Polymers where covalent bonding is present, blended polymers are cre-
ated by physical mixing of two or more polymers. Copolymers
Organic polymers in the form of solutions or melts are the most and polymer blends are readily employed to attain hybrid physic-
frequent employed materials in electrospinning. In recent years, ochemical and mechanical properties. Although consistency
over two hundred polymers have been successfully fabricated and reproducibility among batches to produce homogenous
into fibers and applied in various fields.[100] Based on their occur- fibers of desired morphology will require optimization of the
Table 3. Overview of recent studies utilizing green, environmentally safe, and biorenewable solvents for electrospinning.
Solvent system Polymer (additives) Electrospinning technique Ref.
2-Methyltetrahydrofuran (2MeTHF)/formic Poly(3-hydroxybutyrate-co-3-hydroxyvalerate Mono-axial (using a syringe heater, to [87]

acid (PHBV) prevent sol-gel transition)
Acetic acid/ethyl acetate/water Polycaprolactone (PCL) + gelatin Mono-axial (blend) [88]
Acetic acid/formic acid/acetone PCL Needleless (AC) [89]
Acetic acid/water Cellulose acetate (CA) and chitosan (CS) Co-axial electrospinning [90]
Ethanol Ethanol-soluble polyurethane (TPU) and In situ (handheld) [91]
thymol (antibacterial compound)
Ethanol Polyvinylpyrrolidone (PVP) Needleless (wire) [92]
Ethanol/diacetone alcohol Polydimethylsiloxane (PDMS) and Mono-axial [93]
polyamide pellets
Ethanol/water Chitin propionate and PEO Mono-axial (blend) [94]
Ethyl acetate/acetic acid Ethylcellulose polyglycerol polyricinoleate Mono-axial (emulsion) [95]
(surfactant) + polyethylene glycol (PEG)
Dimethyl carbonate (DMC)/water Polylactic acid (PVAc) + Mono-axial [96]
tetrabutylammonium bromide (TBAB,
salt)
Dimethyl sulfoxide (DMSO)/acetone Polyacrylonitrile (PAN) Centrifugal [97]
DMSO/acetone Polyvinylidene fluoride (PVDF) + LiCl Mono-axial [98]
(additive salt)
Methyl ethyl ketone (MEK)/formic acid PHBV Mono-axial (using a syringe heater, to [87]
prevent sol-gel transition)
Water Polyethylene oxide (PEO) Needleless ultrasound-enhanced [99]
electrospinning (USES)
parameters mentioned above, in concept, the predominate num- weight, high molecular chain rigidity, and poor solubilities asso-
ber of organic polymers can be electrospun in the presence of ciated with the ICPs. At the same time, the increased solution
a suitable solvent (for polymer solutions) or by obtaining melts conductivity can overly increase the level of charge distribution,
without thermal degradation (for polymer melts). facilitating jet instability.
The nature of the polymer will have a direct effect on
the properties of the fibers. Selecting the appropriate poly-
mer for the application of interest is an indispensable step. 3.4.2. Small Molecules
Synthetic polymers for electrospinning are generally chosen
based on thermal behavior and molecular force properties Chain entanglement can control molecular motion and disrupt
with thermoplastics (e.g., polyesters, polystyrene [PS], polyvinyli- the free movement of molecular segments, thus influencing
dene fluoride [PVDF], nylon-6, among others), thermosets a polymer’s rheological, morphological, and mechanical prop-
(e.g., polyurethane [PU], polymethyl methacrylate [PMMA], erties. Increasing the degree of chain entanglement can re-
among others) and elastomers (e.g., polyurethane [PU], polyg- duce the effect of Rayleigh’s instabilities and maintain a stable
lycerol sebacate [PGS], among others), all readily electro- jet.[105] Thus, under the appropriate conditions, small molecules
spun. For biomedical applications, biopolymers are classi- that can self-assemble in the presence of the appropriate solu-
fied based on their origin to natural (e.g., proteins,[101] nu- tion conditions (for instance, through anionic or non-anionic
cleic acids,[102] and even polysaccharides[103] ) and synthetic, noncovalent bonding) may attain sufficient chain entanglement
which can be subcategorized into non-biodegradable (e.g., to be electrospun into fibers. In addition, the self-assembled
polyvinyl chloride [PVC], polypropylene [PP], among oth- structures of molecules can be stable in solutions or melts
ers) and degradable (e.g., polycaprolactone [PCL], polylactic when adequate intramolecular interactions form. Among the
acid [PLA], poly(ethylene oxide) [PEO], polyvinylpyrrolidone small molecules successfully electrospun are phospholipid am-
[PVP], among others). Aliphatic polyesters intrinsically con- phiphiles, monopeptides, dipeptides, tetraphenylporphyrin com-
ductive polymers (ICPs) have also been successfully electro- pounds, and cyclodextrins.[106–109] In instances where a small
spun to develop flexible electronics, conductive coatings, energy molecule cannot produce stable intramolecular interaction to
nanogenerators, supercapacitors, batteries, and biosensors.[104] obtain the required chain entanglement, carrier polymers may
ICPs like polypyrrole (PPy), poly(3,4-ethylenedioxythiophene)- be incorporated into the polymer mixture and subsequently re-
poly(styrenesulfonate) (PEDOT:PSS), and polyaniline (PANI), moved through postfabrication strategies (e.g., solvent or heat
have been electrospun in the presence of carrier polymers, as treatment). Another way that small molecules can be manipu-
blends. In the case of ICPs, incorporating a carrier polymer is lated into fibers is through in situ polymerization approaches,
generally considered a sine qua non to improve the low molecular such as photopolymerization.[110]
3.4.3. Composite Materials In recent years, M&S has focused on improving the consis-
tency of the process and the likelihood of attaining invariable
Many state-of-the-art fibrous materials are forged from com- fiber morphological traits, as well as understanding the electric
posite polymer blends based on sol-gel chemistry principles. field intensity and distribution based on spinneret configuration
While polymer–polymer composites, where polymers of differ- (e.g., needleless cylindrical systems) and collector shape.[112]
ing physicochemical characteristics can produce peculiar com- A technological constraint that continues to exist today is hav-
posite fibers that bring together their distinct properties (such ing physical control over the fiber diameter and attaining a low
as, adjustable biodegradability and biocompatibility along with standard deviation. Although empirical findings can determine
mechanical stability), incorporating colloids in a polymeric so- to a great extent, variations in fiber diameter based on solution
lution can be implemented to immobilize nanomaterials within composition and electrospinning properties, to date, there is no
the fiber configuration. Colloids are good examples of polymer- library encompassing the extensive experimental work that has
particle composite electrospun structures that rely on the parti- been carried out in the field over the years. Taking advantage of
cles’ aggregation state within a solution during electrospinning. the vast number of trial-and-error studies conducted, M&S, could
A stable jet can be maintained when sufficient polymer entangle- ultimately provide an accurate, predictive tool utilizing a verified
ment and particle distribution are present, allowing composite model that considers the wide range of experimental parameters.
fibers to form.[58] To produce electrospinnable solutions consist- The response surface methodology (RSM) is a statistical poly-
ing of polymer–colloid systems, in general, a less viscous solu- nomial method that explores the relationships of several explana-
tion of lower concentration and higher molecular weight, along tory and response variables to demonstrate and analyze existing
a compatible solvent system of lower conductivity, to account relationships. RSM aims to optimize the response of output vari-
for the addition of the desirable compound, is required. Typi- ables by influencing the responses of several independent in-
cally, the material is first dispersed in a polymer-compatible sol- put variables.[113] RSM, along with machine learning regressions
vent and homogenized trough ultrasonication before being in- (MLR); a method used to investigate the relationship between in-
troduced into the polymeric mixture and vigorously stirred. The dependent variables and a dependent variable or outcome. Both
morphology of the composite fibers will be affected by the criti- RSM and MLR can be valuable predictive tools, reducing the need
cal value of the average particle diameter and its impact on the for unnecessary experimentation when an optimal set of param-
polymer solution’s properties, such as conductivity and viscosity. eters with a high degree of confidence can be computed.[114]
Through this process, a variety of materials and substances can RSM has been extensively studied with regard to obtaining
be successfully incorporated into a fiber configuration, including consistent fiber diameters,[115] tunable fiber orientation,[116] pore
carbon, organic and inorganic 0D, 1D, 2D, and 3D nanostruc- size and fiber quality,[117] and determining the number of beads
tured materials, as well as pharmaceutical compounds. Table 2 and bead size.[114] Interpolation machine learning models, such
provides a comprehensive list of the parameters that need to be as Kriging,[118] artificial neural networks (ANNs),[119] and grey-
met for consistent electrospinning and homogeneous fiber for- correlation analysis (Grey theory),[120] are powerful tools in un-
mation. derstanding unknown nonlinear processes. These methods have
Although significant efforts have been directed towards achiev- provided insightful studies focused on determining and analyz-
ing intricate fibrous membrane properties by manipulating the ing fiber diameter.[121]
produced membranes during electrospinning (e.g., a coagula- Theoretical modeling, along with experimentation, can be vi-
tion or oxidizing bath collector), or post-fabrication (physical or tal in better understanding the variant processes described in the
chemical), including surface modification (e.g., grafting), in situ following section, and by doing so, can significantly improve re-
polymerization, plasma treatment, carbonization, physical va- producibility and fiber output.
por deposition, sputter coating, electrospraying, among other,
the subsequent sections of this review will exclusively focus on
apparatus-specific technological advancements. 3.6. Classification
The electrospinning techniques introduced in this review are

categorized based on spinneret configuration into two groups:
3.5. Predictive Modeling
needle-based and needleless. Six needle-based electrospinning
techniques (mono-axial, co-axial, tri-axial, centrifugal, 3D, and
As a critical design tool, modeling and simulation (M&S) has
handheld electrospinning) and five distinct needleless high-
played a tremendous role in understanding the complex inter-
throughput technologies (roller, bubble, corona, wire, and high-
dependent events that collectively make electrospinning feasible.
speed electrospinning) were identified and are summarized in
Prediction models, where experimental work falls short, can pro-
Table 4 below.
vide important insights about the underlying processes, as well
as reduce unnecessary trial-and-error experimentation, thus sav-
ing resources (e.g., significantly reducing the use of solvents). To- 4. Advanced Electrospinning Technologies:
day’s understanding of the polymer solution properties, external Needle-Based
forces affecting the electrospinning process, as well as the for-
mation stages; Taylor cone, jetting, elongation, jet instability, and 4.1. Mono-Axial
solidification, would not have been possible without the collective
efforts of several research groups providing those mathematical Introduced by Cooley and Morton in 1902, mono-axial is the first
models.[111] and most commonly used electrospinning method that evolved
Table 4. Classification of electrospinning techniques. distance), the linear region between the spinneret and the col-
lector. As the jet expands toward the collector, it becomes thin-
Needle-based Needleless ner, resulting in the rapid evaporation of the solvent, leaving
• Mono-axial • Roller
behind solid polymer fibers to be deposited on the collector.[53]
Variations of the mono-axial electrospinning setup include linear
• Co-axial • Bubble
or circular motion multi-spinneret systems consisting of mul-
• Tri-axial • Corona tiple mono-axial needles.[122] This approach has been reported
• Centrifugal • Wire to be ineffective for the high-throughput production of NFs due
• Three-dimensional (3D) • High-speed to electrostatic interactions between nearby needles and needle
• Handheld (in situ) clogging, although it is still employed by some high-throughput
electrospinning systems today. The most important advantages
and disadvantages of mono-axial electrospinning can be found in
Table 5.
To some extent, the limitations associated with the fact
from electrospraying.[26,27] As previously described, a conven- that mono-axial electrospinning can only be used to pro-
tional mono-axial setup consists of a high-voltage power supply, duce fibers derived from a single solution can be circum-
a syringe container with a single metallic hollow capillary (blunt vented via sequential electrospinning, co-electrospinning, or
metallic needle), and a counter electrode collector placed at a spe- electrospinning-co-electrospraying. Sequential electrospinning
cific distance from the oppositely-charged needle, horizontally or refers to electrospinning solution A for a predetermined
vertically.[103] amount of time, then changing to solution B and continu-
A schematic diagram of the mono-axial electrospinning ing with the electrospinning process onto the same fiber de-
method can be seen in Figure 2a. First, a polymer solution of position, and so on. Co-electrospinning/electrospraying, or con-
predetermined composition is loaded into a syringe and with- current electrospinning and electrospraying, uses a rotating
drawn at a controlled rate using a syringe pump, producing a mandrel as the collector, and two spinnerets fed to two dis-
liquid hemisphere droplet at the tip of a blunt metallic needle tinct reservoirs are placed antiparallel or vertically and hor-
(the spinneret). The electrostatic charges build up at the surface izontally to one another to electrospin/spray simultaneously
of the liquid droplet due to the high voltage applied to the metal- onto the same collector. This simple tweaking of mono-axial
lic needle. When the electric field exceeds a specific value, the electrospinning process can enhance the complexity of the at-
electrostatic forces overcome the surface tension of the polymer tained electrospun mats, producing structures such as layer-
solution or melt, instigating Taylor cone formation from the apex by-layer or mixed membranes that encompass properties de-
of the liquid droplet. Jetting occurs due to the electrohydrody- rived from two or more polymer solutions in a layer-by-layer
namic stresses present in the travel path (referred to as working configuration.[123,124]
Table 5. Advantages and disadvantages of mono-axial electrospinning.
Advantages Disadvantages
1. The spinneret consists of a single needle, making the setup less complex and 1. Limited production capacity. The yield of dry solid fibers via mono-axial
easy to operate. electrospinning is 0.01–0.3 g h−1 , making it suitable only for laboratory use
or projects requiring small fiber outputs, e.g., sensor electronics, where a
thin layer of NFs can be used as interface materials.[ 125]
2. Irrefutably the most well-studied electrospinning method, it can assess the 2. The NFs present a simple structure, presenting a circular cross-section with a
spinnability of new materials and complex composites or optimize the smooth surface. When applied to drug delivery platforms, the lack of a
solution, process, and ambient parameters before production on a large complex fiber structure encourages an initial burst release of the
scale. incorporated compound. Although solvent–drug and polymer–drug
compatibilities can be employed to control the drug release rate,
mono-axially produced NFs perform poorly in sustained release profiles.[ 4 ]
3. Reproducible fine fibers can be obtained in the lower range of the nanoscale. 3. The fabricated scaffolds present a 2D network of small-diameter pores and
In addition, distinct micromorphologies (such as randomly oriented or high pore interconnectivity. The fibrous membranes become too compact
aligned fibers) can be obtained by adjusting the solution, process, and under prolonged spinning periods, often performed to attain mechanical
ambient parameters, the needle’s inner diameter (e.g., gauge), and the type stability. Although overcoming the small pore size constraints associated
of collector (e.g., flat, drum, or liquid bath). with this method can, in some instances, be achieved by postfabrication
processing methodologies capable of widening the pores (such as cryogenic
electrospinning[ 126] and gas-foaming[ 127] ), in general, the pores produced via
this technique are too small for the penetration of large particle and the
majority of mammalian cells.[ 128]
4. Multineedle electrospinning apparatuses capable of facilitating 4. Multineedle electrospinning apparatuses are challenging to operate and
high-throughput production are currently on the market. inconsistent due to electrostatic interactions between nearby needles and
needle clogging.
4.2. Co-Axial Electrospinning ical properties, and the controlled release of defined concentra-
tions of active pharmaceutical compounds or nanomaterials, can
Co-axial electrospinning is a variation of the conventional electro- be fabricated.[132]
spinning method invented by Sun et al. in 2003.[37] Co-axial elec-
trospinning enables independent reservoirs of two different so-
lutions fed onto a co-axial needle to form single composite fibers 4.3. Tri-Axial and Multi-Axial Electrospinning
that present a core/shell morphology.[129] The co-axial spinneret
consists of a double capillary compartment arranged concentri- As the name indicates, the tri-axial electrospinning process uses
cally, with the inner needle fitted within the outer needle. Inde- a tri-axial spinneret made of three concentric needles capable of
pendent solutions travel to the orifice of the co-axial needle from simultaneously infusing up to three different materials. As with
separate pumps, where the flow rates are adjusted accordingly. co-axial, tri-axial electrospinning belongs to the multi-axial elec-
The inner capillary contains the core solution, while the outer trospinning family, with variations reported that include quadrax-
capillary produces the shell polymer.[130] At the orifice, a com- ial and multi-nozzle. Figure 6a shows a typical layout of a tri-
pound Taylor cone forms as the shell polymer solution entraps axial electrospinning setup, which consists of four modules:
the core fluid and is subjected to an applied electric field, concep- three individual solution pumps, a high-voltage power supply, a
tually similar to conventional electrospinning.[59] After the sol- grounded or negatively charged collector, and a spinneret com-
vents evaporate, a heterogeneous but continuous fiber composed prised of three concentric needles. Three pumps are used at ad-
of the core and shell constituents is collected.[131] The basic con- justable feeding rates to drive up to three individual working so-
cept of co-axial electrospinning is illustrated in Figure 5, and the lutions, referred to as outer, middle, and inner. As with all the
limitations and advantages of the technology are summarized in multi-axial technologies, this method can be also employed to
Table 6. electrospin materials that are not solely electrospinnable. The si-
The interactions that govern the properties of the result- multaneous feeding of the three solutions forms a composite Tay-
ing core/shell fibers are determined by the degree of rheo- lor cone when an appropriate voltage is applied to the system.
logical, physical, and chemical dissimilarities between the two Ultimately, trilayer-structured composite fibers can be deposited
solutions.[132] However, a uniformly assembled core/shell fiber on the collector.[131] Foreseeably, all the process parameters that
can only form if a stable Taylor cone is maintained. Process- need to work synergetically to obtain a stable Taylor cone in co-
ing parameters related to co-axial electrospinning have been re- axial electrospinning are applicable in tri-axial electrospinning
viewed in the literature,[133,134] with the studies agreeing that the but at an even greater complexity. For this reason, since multi-
complexity of co-axial electrospinning originates from the dif- axial fibers were first reported in 2009 by Kalra and co-authors,[40]
ficulty in maintaining a stable Taylor cone. To induce a stable only a small fraction of electrospinning research has been fo-
Taylor cone, process parameters should be such that 1) an elec- cused on multi-axial setups, with only 46 articles published since
trospinnable shell solution is used; 2) the shell solution viscos- that date (based on a Scopus search for “triaxial electrospinning”
ity is higher than the core solution viscosity, so that the stress OR “tri-axial electrospinning” OR “multi-axial electrospinning”
relating to the viscosity between the core and shell solutions OR “multi-axial electrospinning AND LIMIT-TO (DOCTYPE ,
overcomes the interfacial tension between them;[135] 3) a low va- "ar")”).
por pressure solvent is used (as fast evaporation may destabilize Figure 6b indicates an SEM image of the trilayer structure.
the Taylor cone); and 4) the conductivity of the shell solution is The trilayer structure adds extra complexity to the properties of
greater than that of the core solution to inhibit core/shell struc- the composite fibers due to the possibility of introducing differ-
tural discontinuities induced by the rapid elongation of the core ent functionalities and compositions through the different layers,
polymer.[132] finding applications in a broad range of fields and, most signifi-
Co-axial electrospinning is an advantageous method since it cantly, in drug delivery.[147] The trilayer structure can function as a
can produce fibers with novel structures out of highly diverse single carrier of multiple substances, adding an extra layer of pro-
polymer pairs (Figure 5d); core–sheath, hollow, and nanoparticle- tection from polymer degradation due to external stimuli.[121] As
decorated, with each component maintaining its separate mate- shown in Figure 6b,c, taking advantage of this concept, compos-
rial identity.[133] By exploiting this feature, sophisticated pairs of ite polymer NFs containing different drugs or variant drug con-
materials can unify their properties into a single composite fiber. centrations can be incorporated within the three-layer format. In
Highly unstable materials, such as enzymes, growth factors, and this regard, the drug concentration will indicate a gradient distri-
rapidly degradable compounds that would otherwise be rapidly bution from the inner core, containing the highest concentration,
broken down within an intricate niche, can be preserved by the to the outer shell, containing the lowest concentration. Further-
sheath material.[136] For this reason, the properties of polymers more, due to the inherent advantages of the trilayer structure,
can be manipulated while employing the co-axial electrospinning under the premise of Fick’s law of free diffusion, the drug re-
technique, which is of interest in the biomedical sector because lease rate from the inner core layer will be further retarded, as
it can be used to develop biocompatible and mechanically stable it must first diffuse through the intermediate layer before reach-
materials.[75] Co-axially electrospun fibers are widely employed ing the sheath, gradually increasing in concentration from the
to develop drug delivery systems that can attain a tailored sub- inner to the outer layer, and thus resulting in extended release,
stance release. Through this process, nanofibrous scaffolds with programmable based on the chemistry of the sheath and the dif-
superior properties to those of monolithic fibers, including a hy- fusability properties of the intermediate layer.[148] Table 7 sum-
drophilic surface within a hydrophobic core, adjustable mechan- marizes the advantages and disadvantages of the process.
Figure 5. Generation of co-axial electrospun fibers. a) Schematic of a standard co-axial electrospinning setup; b) configuration of the co-axial Taylor
cone, following the evolvement of the electrified jet as the voltage amply increases, where polyvinylpyrrolidone (PVP) is the shell and mineral oil is
the core solution;[137] c) schematic representation of the charges forming the co-axial Taylor cone, i) surface charges develop around the surface of
the shell solution, ii) a viscous electrified strain exerts the droplet causing it to be deformed, iii) a stable core–sheath jet develops. d) SEM images of
i) core/shell,[138] ii) hollow,[68] and iii) nanowire-in-microtube structured fibers.[139] Copyrights: (b) Reproduced with permission.[137] Copyright 2017,
Elsevier; (d) (i) Reproduced with permission.[138] Copyright 2019, American Chemical Society; (d) (ii) Reproduced with permission.[68] Copyright 2004,
American Chemical Society; (d) (iii) Reproduced with permission.[139] Copyright 2010, American Chemical Society.
Table 6. Advantages and disadvantages of co-axial electrospinning.
1. Co-axial electrospinning can form novel core–shell fiber structures where the 1. The process is complex. Co-axial electrospinning requires a specialized
activity of the core compound can be protected by the external environment spinneret consisting of two concentrically aligned needles that dispense two
through the sheath material. Core/shell fibers have applications in distinct solutions through two individual syringe pumps. This increases the
nanocatalysis,[ 140] fiber-reinforced composites,[ 141] smart textiles,[ 142] energy complexity of appropriately adjusting the process parameters. Additionally,
storage,[ 143] and filtration[ 110] but predominately for biomedical applications, co-axial needles are expensive to purchase, while cleaning procedures for
such as tissue engineering, drug delivery, and antimicrobial surfaces.[ 4,75 ] clogged needles can be time-consuming and arduous, as needles are not as
often discarded, especially during the early stages of evaluating the
compatibility of the core and shell solutions.
2. Hollow NFs can be formed by selectively removing the core material (e.g., 2. The process is difficult to implement. The core and shell solutions
chemically or thermally) from the core/shell structure post-fabrication.[ 140,144] co-electrospun through a single orifice require good compatibility and similar
physicochemical properties to prevent separation and attain a homogenous
core/shell cross-section.
3. Core/shell drug-loaded fibers can retard the release kinetics of a substance, 3. A balance between the flow rate of the two solutions is required to obtain a
preventing the initial burst release commonly associated with monolithic homogenous distribution of the shell component within the core–shell
fibers. This way, different controlled-release drug delivery systems requiring structure. However, achieving this balance can be difficult as it requires
substantially smaller concentrations of a given substance can be attained. tuning of the interfacial tension, viscosity, solvent volatility, and conductivity
Although the core/shell chemistry and surface properties can be modified between the two independent solutions to ensure comparable flow rates.
depending on the desired release mode, in general, the drug loaded into the Differences in the extrusion rate will result in inhomogeneous compound
core compartment of the structure is released by permeation through the fibers. For example, a low shell flow rate may disrupt fiber formation, whereas
outer shell of the polymer fiber and degradation of the shell.[ 145] a higher flow rate produce a fragmented sheath structure.[ 146]
4. This process makes it feasible to electrospin materials that are not
electrospinnable per se due to their chemistry (such as oligomers) by
accommodating them within the fiber’s core if the core and shell solutions
are sufficiently compatible.
4.4. Centrifugal Electrospinning When the combined forces overcome the polymer droplet’s sur-
face tension and viscous resistance, jetting initiates and ultrafine
Centrifugal, or rotary jet, electrospinning (CES) is a modified NFs form. The facile mechanical rotation and lower voltage re-
technique that combines electrospinning and centrifugal spin- quirements make CES the best-reported technique for achieving
ning principles (Figure 7 and Table 8). In traditional centrifugal highly aligned NFs.
spinning, spinning is initiated by the centrifugal force acting on Recently, Norzain and Li[153] proposed a mathematical model
the jet, which is influenced by the mass of the polymeric solu- based on Newton’s second law taking into account the several
tion, the angular velocity, and the radius of the centrifugal disc forces the polymeric jet is subjected to during CES; centrifugal
(the distance between the spinneret and the collector).[153] force, electrostatic force, surface tension force, and viscous force.
The first CES apparatus was created by Andrady et al.[38] in As reported in two publications, Erickson et al. have developed
2005. A CES apparatus consists of a rotary feeding plate (spin- highly uniform (based on the fiber diameter standard deviation),
neret), a high-voltage power supply, a feeding channel, a motor, uniaxially aligned, chitosan (CS)-PCL and hyaluronic acid-coated
and a collector. The key feature of this technology is the use of a NFs, illustrating the importance of fiber orientation in influenc-
high-speed motor to rotate the spinneret and, in some instances, ing tumor cell motility and tissue topography.[155,156] Works by
the collector. Following the same electrospinning principles, high Wang et al.[157,158] explored the effects of dual-rotation CES, where
voltage is applied between the rotary feeding plate and the collec- both the spinneret and collector rotate in the same, counter,
tor. The spinneret consists of needles evenly distributed around or multidirectional orientation while assessing a range of poly-
the edges of a disk, although needleless rotating spinnerets have mers: PVP, polystyrene, PCL, and thermoplastic polyurethane
also been reported in the literature.[154] The collector can be a (TPU) toward the development of complex drug release ma-
cylindrical stationary plate where fibers are deposited horizon- trices, based on the fiber’s morphological properties. Yanilmaz
tally in a downward or upward motion, or a ring/multiple-pole and Zhang[159] used this technique to develop polyacryloni-
circularly-arranged metal strips/wires collector surrounding the trile/polymethylmethacrylate (PAN/PMMA) carbonized NFs as
spinneret, where fibers are collected either in a static or mo- a separator material for Li-ion batteries. The authors reported
tion mode. As the polymer is fed into the spinneret, the spin- that compared to microporous polyolefin membranes, the cen-
neret’s rotation speed must be appropriately adjusted to allow for trifugally electrospun PMMA/PAN membranes presented bet-
Taylor cones to form at the end of each needle as the solution ter ionic conductivity, higher electrochemical oxidation limit, and
is evenly extruded and electrified. The synergetic effect of cen- lower interfacial resistance coupled with lithium.
trifugal and electrostatic forces governs the formation of Taylor Among the notable attempts to improve the process param-
cone, resulting in higher production rates of fiber than the con- eters, Valipouri et al.[160] developed an air-sealed setup that im-
ventional electrospinning method while requiring a lower work- proved the stability of the jet, a commonly reported issue of
ing voltage or rotating velocity than the individual techniques. CES. Kancheva et al.[161] achieved radial fiber deposition of highly
Figure 6. The tri-axial electrospinning process. a) Tri-axial spinneret: i) Illustrative diagram of the setup; ii) SEM image of a trilayer structure. Adapted
from ref. [147]. b) Transmission electron microscopy (TEM) cross-section depiction of tri-axial fiber loaded with two different substances, consisting of
a PVP core loaded with Keyacid Blue (blue particles), a PCL intermediate layer, and a PCL outer layer loaded with Keyacid Uranine (yellow particles).
Adapted from ref. [149]. c) Schematic depiction of a dual drug release system of the same substance. This system consists of a burst release (42% of
the loaded drug within 2 h) of ketoprofen through a water-soluble outer sheath (PVP) and the subsequent sustained release (90% of the loaded drug
within 60 h) of ketoprofen-loaded CA core by retarding its release through an intermediate layer of blank CA. Adapted from ref. [150]. Abbreviations: PVP,
polyvinylpyrrolidone; PCL, polycaprolactone; CA, cellulose. Copyrights: (a) Adapted with permission.[147] Copyright 2015, American Chemical Society;
(b) Adapted with permission.[149] Copyright 2013, American Chemical Society; (c) Adapted with permission.[150] Copyright 2020, Elsevier.
Table 7. Advantages and disadvantages of tri-axial electrospinning.
1. Tri-axial electrospinning has distinct advantages over other electrospinning 1. The design of the concentric spinneret plays an essential role in the success
methods due to its ability to form complex multilayer nanostructures. By of the process: variations in the intraneedle spacing and inner diameter
alternating the physicochemical properties of each layer, this methodology between the concentrically aligned needles can positively or negatively affect
finds applications in tissue engineering, where mechanically durable the distribution of each material within the compound fiber during Taylor
synthetic materials can be integrated within the core structures, allowing cone formation and jetting.[ 152]
naturally derived materials, which may lack mechanical stability, to be
included in the outer layer, enhancing, for instance, cell adherence and
proliferation.[ 147,151]
2. Tri-axial electrospinning can overcome problems associated with limited drug 2. The quality of the spinneret. A good tri-axial spinneret must be durable to
solubility. This method can be used to load sensitive substances such as obtain reproducible results by withstanding harsh washes and erosion from
small molecules, proteins, and growth factors that may present inadequate solvents.[ 53 ] Furthermore, the electrical distribution through the outer needle
drug release kinetics and be sensitive to pH fluctuations and the presence of material must be sufficient and stable enough to electrify the composite fluid
harsh media. In such instances, tri-axial fibers could allow for the release of at the point of eruption.
the desired compound to the appropriate tissue site (e.g., a tumor).[ 148]
3. Tri-axial electrospinning can create tunable drug release kinetics and 3. General difficulties of implementation. It can be challenging and, in many
transport mechanisms, such as multistep diffusion drug delivery systems. instances, improbable to attain three compatible spinning solutions with
Tri-axial fibers can incorporate multiple single-substance drug release profiles similar physicochemical properties to prevent separation. Even if that is
or the possibility of loading variant substances in each compartment.[ 149,150] feasible, it is exceedingly difficult to synchronize the inner, intermediate, and
This way, for instance, combining an initial burst release (e.g., outer flow rates to form a well-distributed compound Taylor cone and keep
immediate-release and first-order systems) with a controlled-release profile the concentric structure continuous through the entire process, primarily
(e.g., zero-order release) is feasible. due to gravity and surface tension effects.
Figure 7. Centrifugal electrospinning. a) Schematic of the CES process. b) Diagram depicting the electric repulsion and centrifugal forces that work
synergetically to overcome the solution’s surface tension at the spinneret’s surface and induce fiber formation. A rotating disk, attached to a motor
comprised of multiple pits (spinneret exits), discharges polymeric solution at a controlled rate via a syringe pump system. An applied voltage and
the rotational velocity of the disk facilitate the formation of multiple Taylor cones, which, via high frequency of rotation, expand to form ultrathin fibers.
Reproduced from ref. [164]. c) Development of aligned multicompartment composite microfibers at 120 g h−1 production rate. On the left is a schematic
of the CES setup consisting of a double solution reservoir at the spinneret and an iron wire ring collector. On the right is a fluorescence image indicating
the successful production of blended aligned fiber configurations. Abbreviations: Ω, angular velocity; Fcen , centrifugal force; Frep , electrostatic repulsion;
Fatt , attraction toward the collector; Fair , guiding air. Reproduced from ref. [158]. Copyrights: (b) Reproduced with permission.[164] Copyright 2020,
American Chemical Society; (c) Adapted with permission.[158] Copyright 2018, Springer Nature.
Table 8. Advantages and disadvantages of centrifugal electrospinning.
1. Ultrafine alignment in the micro- and nanoscale can be attained much more 1. CES is a relatively new method, with approximately a hundred articles
straightforwardly than through conventional electrospinning due to the published. Due to the integration of a centrifuge compartment, the design
combined effect of electrostatic and centrifugal forces. Furthermore, in and development of CES (especially toward the spinneret and collector
general, the process requires lower jet initiation voltage and rotating speed, configuration) are more complex. As such, during CES additional process
which can improve the operational safety of the process by reducing injuries parameters must be investigated and optimized for successful fiber
associated with high-voltage and high-speed centrifugation.[ 160] production.[ 141]
2. CES primarily produces loosely packed microfibrous structures that display 2. One of this method’s limitations is the difficulty of incorporating active
fiber directionality with larger mean pore sizes.[ 165] This can find applications substances due to the absence of a complex hierarchy.[ 166] Early reports of
in tissue engineering and scaffold development. co-axial CES fibers have recently been published,[ 163] but further research is
required.
3. CES can be used to electrospin higher concentration solutions, and polymer 3. The majority of CES reserach has concentrated on spinneret configuration
melts through the additional centrifugal forces applied into the system, using mon-axial needle or needle-like arrays designs. Although due to the
assisting fluid transport where jet initiation may not be feasible due to centrifugal forces and the ability to distribute the individual nozzles in a 360°
increased viscosity. format, near-electric field effects are not considered an issue, nozzle clogging
and off-target fiber jetting can still occur (especially toward nearby needles),
making the process laborious to set up and clean.
4. Capable for scale-up. A higher fiber production rate is feasible due to the
synergetic effect of the two processes, allowing jetting to occur at increased
extrusion rates and through the ability to collect fibers in a 360° collector
configuration.[ 141] In addition, needleless CES is feasible, although further
research is needed.
Figure 8. 3D electrospinning technologies. a) 3D electrospinning setup combining conventional electrospinning and 3D printing, i) schematic illustra-
tion of the setup; ii) photograph of the 3D electrospinning device; iii) schematic representation of the device aspects of the apparatus; iv–v) obtainable 3D
structures; vi) SEM image of the 3D deposited fibers. Adapted from refs. [169,170]. Schematic of the b) wet electrospinning and c) cold-plate electrospin-
ning technique. Adapted from ref. [171]. d) Photograph comparing 3D fibrous scaffolds produced by salt-leaching electrospinning (SLE) and cold-plate
electrospinning (CPE). Modified from ref. [50]. Copyrights: (a) (i) Reproduced with permission.[169,170] Copyright 2020, Elsevier; (a) (ii–vi) Adapted with
permission.[169,170] Copyright 2021, Elsevier; (c) Reproduced with permission.[171] Copyright 2016, Elsevier; (d) Adapted with permission.[50] Copyright
2015, Elsevier.
aligned fibers (fiber diameter 550 ± 90 nm) and produced elec- ity to develop a highly porous 3D structure, which can benefit
trospun mats with a large area (2200 cm2 ) within 20 min. In fields such as complex 3D tissue models with improved cell infil-
this work, fiber alignment was achieved when using circularly- tration, and wound healing[143] (Figure 8 and Table 9).
arranged metal strips as the collector but not with a cylindrical Initially, significant research focused on postprocessing, mul-
collector (at a rotating speed of 1900 rpm). Chang and co-workers tilayering, and template-assisted electrospinning techniques to
studied the effects of a viscoelastic jet during CES and mathe- obtain 3D built-ups.[66] Postprocessing techniques involve pro-
matically described, through dimensionless number and group ducing 2D electrospun membranes and folding, freeze-drying,
analysis, that the strong stretching force and a fast extension and gas-foaming the structure to create a 3D version from 2D
speed obtainable during the process can significantly reduce the electrospun mats. As the name suggests, multilayer electrospin-
effect of the whipping instabilities and fabricate a series of uni- ning involves compiling multiple layers of sequential electro-
axially aligned polymeric NFs with improved physical properties spun or co-electrospun materials. Finally, the template-assisted
such as high modulus, hardness, crystallinity, and good molec- method consists of electrospinning onto a sacrificial 3D tem-
ular orientation.[162] For the first time, Gu et al.[163] recently ad- plate, such as mechanical and matrix templates, which subse-
dressed the development of complex NF structures via the CES quently leached (postprocessing), leaving behind a 3D fibrous
technique by integrating CES with co-axial electrospinning to structure. Nonetheless, although these approaches have seen sig-
produce core–sheath structures out of poly(vinyl alcohol) (PVA) nificant recognition in the literature, they cannot be considered
(core) loaded with paclitaxel and poly(l-lactic acid) (PLLA) (shell), 3D electrospinning technologies, as they cannot directly produce
with a controllable drug release profile by adjusting the thickness 3D electrospun structures.
of the sheath material. Two variations of conventional electrospinning, i.e., wet
and cold-plate electrospinning, and one self-assembly-inspired
electrospinning apparatus that integrates 3D printing and
4.5. 3D Electrospinning electrospinning principles to produce CAD-assisted 3D mi-
cro/nanofibrous configurations, are the only technologies, to
A significant restraint of conventionally produced electrospun date, capable of instantaneous one-step production of 3D elec-
membranes is their inherent 2D structure. This hinders the abil- trospun structures (Figure 8a).
Table 9. Advantages and disadvantages of 3D electrospinning.
1. It is one of the most straightforward and advanced techniques to 1. Nano-microfiber blocks made by 3D electrospinning are soft and fluffy
manufacture 3D structures with tunable morphology, pattern, and physical (woven); they have cotton-like structures when they are dry but often break
and chemical properties. down upon contact with a liquid, posing an issue for anisotropic lamellar
deposition.
2. Due to non-contact operation and CAD-directed spinneret motion, 3D 2. Polymer systems with higher conductivity are necessary for 3D assembly,
electrospinning is the only reported technology capable of directing the hence narrowing the class of materials that can be used.
morphology of the 3D structures without requiring subsequent
post-fabrications steps.
3. Waste produced is reduced via 3D electrospinning, as it does not require 3. Increasing the height of the constructs decreases the precision of the
post-fabrication procedures to obtain 3D scaffolds. process, limiting upscaling.
4. CPE can produce nonwoven, microporous structures with better mechanical 4. 3D electrospinning methodologies such as CPE, are limited to water-soluble
stability than 3D electrospun structures. polymers, require significant post-fabrication processing and can only attain
random 3D macro-architectures. Similarly, wet electrospinning is limited by
the range of coagulation solvents available for a specific polymer.
Furthermore, the depth of the bath (from the bottom where the electrode is
placed to the bath’s surface) limits the upscaling of the process and the
ability to produce diverse 3D structured macromorphologies.
Yokoyama and co-authors first described the wet electrospin- spun structures, was developed. 3D electrospinning is the first
ning technology in 2009 as a novel method capable of fabricat- technology that combines electrospinning and extrusion-based
ing 3D spongiform NFs.[44] The process is conceptually similar to 3D printing to develop CAD-assisted 3D fibrous patterns.[51]
conventional electrospinning, with the key difference being the Vong et al.[51] first described this technology in 2018, demon-
use of a bath as the collector filled with a low surface tension strating the controlled deposition of 3D buildup by including a
solvent (e.g., tertiary-butyl alcohol), which is capable of solidi- conductive additive in the electrospinning solution (H3 PO4 ). It
fying and attracting the formed fibers [e.g., poly(glycolic acid)], is a non-contact printing technique suitable for fabricating com-
toward a grounded metallic plate placed at the bottom of the plex and nonplanar surfaces. Complex electrospun 3D structures
bath (Figure 8b). This process produces nonwoven 3D structures benefit from various biological, mechanical, and mass transport
that are relatively short, with a low bulk density and high poros- properties. A 3D electrospinning setup possesses a high-voltage
ity. Following the same principles, Ghorbani et al.[167] produced source and solution controller with a fused deposition model-
PLA porous 3D scaffolds in a sodium hydroxide (NaOH) bath for ing 3D printer, which provides the x-y-z motion control. The
wound healing applications. Zhang et al.[150] employed this tech- polymeric solution is fed into the moving nozzle, connected to
nology to produce Rana chensinensis skin collagen (RCSC)/poly(ɛ- a high voltage that allows the directed deposition of 3D struc-
caprolactone) (PCL) Ag nanoparticle-loaded in an ethanol bath, tures. The guided NF assembly process forms these structures
creating 3D porous nanofibrous materials with ≈90% porosity. into shapes due to electrostatic induction, rapid evaporation,
Sheikh et al.[50] described the cold-plate electrospinning tech- and polarization.[146] In follow-up work, Vong et al.[169] analyzed
nique in 2015 when they produced 3D silk fibroin large- the mechanism behind the 3D buildup, demonstrated that the
pore nanofibrous scaffolds (Figure 8c,d). During cold-plate elec- incorporation of electrodes can further enhance the shape of
trospinning, as the name suggests, a collector plate is placed over the produced structures at the collector’s surface, and demon-
a heat transfer pipe connected to an immersion chiller that can strated the upscaling of the process, creating 3D macrostructures
lower the plate temperature to −90 °C, at which ice crystals form, up to 5 cm in height out of polystyrene, polyacrylonitrile and
enhancing the conductivity and subsequently instigating the de- polyvinylpyrrolidone within 10 min.
position of the fibers in a layer-by-layer format. In this work, silk
fibroin was blended with PEO, where the scaffolds produced were
subsequently freeze-dried, immersed in ethanol for crystalliza- 4.6. Portable Electrospinning
tion, and finally immersed in deionized water to remove the car-
rier polymer (PEO). The 3D scaffolds improved cell infiltration in Portable electrospinning refers to handheld and lightweight elec-
vitro (using human dermal fibroblasts and keratinocytes), com- trospinning devices designed to produce fibers on-site (Figure 9
pared to the NFs obtained using conventional electrospinning and Table 10). The technology was inspired by wound care
due to the higher porosity and larger pore sizes attained via this and management as an alternative approach to simultaneously
methodology. achieving hemostasis, wound protection from infection, and pro-
Although the above technologies can produce 3D struc- moting tissue regeneration.[172] The inspiration behind the de-
tures through electrospinning and have gradually evolved velopment of in situ fiber deposition onto a wound was trans-
since they were first introduced in 2005,[143] after subsequent duced by this approach being able to provide painless personal-
exploration,[168] 3D fibrous self-assembly via electrospinning, an ized deposition of lightweight dressings directly on the injured
exciting single-step fabrication method of producing 3D electro- site.[66] The initial drawback of the portable electrospinning de-
Figure 9. Portable electrospinning apparatuses. a) A representative depiction of a portable electrospinning device. i) Schematic diagram of its compart-
ments; photographs of ii) jetting and iii) in situ fiber deposition onto a hand. Adapted from ref. [174]. b) A schematic diagram of a portable melt-extrusion
electrospinning device. Adapted from ref. [183]. c) A photograph of the commercially available portable electrospinning device, currently undergoing
clinical trial for its application in wound management (Spincare, Nanomedic, Israel). d) A 3D-printed apparatus. i) A rendered image of the CAD de-
sign; ii) a schematic of the electrospinning assembly, consisting of the 3D-printed compartments, a 12 V battery, a high-voltage converter, conductive
wires for HV output, a syringe, and a metallic needle. iii,iv) Photographs of the assembled device. Adapted from ref. [182]. Copyrights: (a) Adapted with
permission.[174] Copyright 2015, Royal Society of Chemistry; (b) Adapted with permission.[183] Copyright 2020, Springer Nature; (c) Reproduced from
Nanomedic Technologies Ltd.; (d) Reproduced with permission.[182] Copyright 2020, Frontiers.
vice first designed by Sofokleous et al. in 2013 was the require- within PVP blends.[178] Dong and co-workers used a hand-
ment of a cord to power the high-voltage power supply, thus held electrospinning device to electrospin a PCL blend incor-
minimizing its accessibility and the notion of onsite use.[173] Xu porating aggregation-induced emission luminogens, a newly
et al. were the first to resolve this issue by miniaturizing an emerged group of photosensitizers able to generate reactive oxy-
electrospinning apparatus by integrating a battery power source, gen species, for the treatment of multidrug-resistant bacterial
producing a device with dimensions of 10.5 × 5 × 3 cm3 , only infection.[179] Earlier this year, Xu et al.[180] described for the
weighing ≈120 g, naming it battery-operated e-spinning appara- first time the in situ electrospinning of PVA NFs incorporat-
tus (BOEA). The compact structure produced fibers in a cordless, ing bone marrow-derived stem cells (BMSCs) using a hand-
single-hand motion.[174] They were able to electrospun N-octyl-2- held apparatus for the treatment of non-healing wounds. Zhang
cyanoacrylate (hemostatic glue) with a range of polymers; PCL, et al.[181] developed a simple portable electrospinning device
PS, PVP, PLA, and PVDF. Subsequent apparatuses inspired by consisting of a syringe, a metallic needle, and a AA battery-
these findings further miniaturized the electrospinning equip- powered high-voltage converter (where a 3 V battery can pro-
ment and focused on evaluating in situ wound healing repair in duce a 10 kV output) to in situ electrospin core/shell nanoparti-
animal models.[175–177] cles (NaYF4:Yb/Er@NaYF4:Nd@hypericin, 50 nm in diameter)
Several antibacterial polymer formulations have been suc- blended with PVP dissolved in acetone (≈500 nm in diameter), to
cessfully electrospun using handheld apparatuses to produce be used for photodynamic therapy; a type of treatment that can
wound dressings, including PCL loaded with silver nanoparti- generate reactive oxygen species (ROS) to effectively eliminate
cles mesoporous silica nanoparticles (AgNP) and asymmetri- bacteria under light irradiation.
cally spun PVP iodine-loaded NFs (HHE-1; handheld portable Portable electrospinning has encouraged the establishment
electrospinning apparatus, Qingdao Junada Technology Co., of an Israeli-based company, Nanomedic, which has success-
Ltd.).[177] Recently, the same device has been used to de- fully commercialized a handheld electrospinning device, Spin-
liver active herb extracts (Lianhua Qingwen Keli) incorporated Care. The equipment is currently undergoing clinical trial for the
Table 10. Advantages and disadvantages of portable electrospinning.
1. Handheld battery-powered electrospinning devices are the only reported 1. This is quite a new technology, with only a handful of patents filled and 25
apparatuses capable of producing electrospun fibers on the spot. This gives research articles published to date. The equipment design is complex,
the device distinct advantages in medical applications, especially in wound particularly in regards to ensuring patient compliance and safety with
management, where fibers incorporating pharmaceutical compounds, regulations.
growth factors, or even cells can be directly deposited in a layer-by-layer
format in an open wound. In this way, patients have reported alleviated pain,
while the most recent in vivo studies and ongoing clinical trials show
promising results.[ 66 ]
2. By formulating and depositing the fibers on-site, the technology can be 2. In general, the production of in situ electrospun fibers is challenged by poor
considered more economically friendly by limiting excess fiber deposition. It stability during the fabrication due to the inability to retain consistent
is also beneficial for unstable substances that may not survive prolonged spinning, applying opposite potential charge (always grounded, with no
storage periods, post-fabrication treatments, or sterilization protocols. collector), and working voltages that do not exceed 10 kV. These issues often
result in inconsistent fiber morphologies of a single material of low
histocompatibility. Improvements concerning the reproducibility, quality,
purity, potency, and solvent toxicity of the fibers produced are required.
3. As a portable technology capable of rapidly producing lightweight dressings, 3. Currently, only a limited number of materials, mostly water-soluble, have
it can be utilized by emergency medical services, fire and rescue services, and been electrospun through this process, due to the limited selection of
the military. solvents and additives . It is necessary to produce a wider range of naturally
derived and synthetic polymers through this process to gain better
undertsanding of the process parameters. Further improving the devices’
interface will be required to eliminate issues with residual solvents.
external treatment of burns and wounds, and as of this year, free-surface electrospinning is an alternative method of high-
44 participants have enrolled. Five case studies have been made throughput production of fibers with no constraints of clogged
available, including the treatment of a graft donor site area and needles, providing freedom over the spinneret’s configuration.
partial thickness burns (clinical trial: NCT02997592). In 2004, Yarin and Zussman initially described the produc-
Recently, Chen and co-authors[182] fabricated a 3D-printed tion of free-surface NFs by placing a layer of polymer solution
handheld apparatus consisting of three compartments; a cover, underneath a magnetic liquid that was overlapping a permanent
a handle, and the main body using Objet350 Connex 3D. The magnet against a vertically placed oppositely charged magnet by
authors made the standard template library (STL) files publicly applying high DC voltage.[19] A year later, Jirsak and co-workers
available. Upon assembly, the handheld electrospinning device patented a process in which a rotating charged electrode, im-
was powered by a 12 V rechargeable Li battery (acting as a volt- mersed within a polymer solution, placed underneath a counter
age generator), capable of producing up to 10 kV DC high voltage. electrode, could fabricate NFs at an increased production rate, in
A high-voltage inverter was connected to metal shrapnel through an upward bottom-up motion, with the assistance of an airstream
a lead wire and was used to electrify the stainless-steel spinneret to increase the auxiliary drying efficiency of the system.[24]
needle. The polymer solution was extruded through a syringe us- Lukas et al.[186] developed an electrohydrodynamic theory that
ing a “gun motion” (finger extrusion) and was attained via a pis- describes the self-organization of electrified liquid jets from an
tol palm extrusion introduced to high-voltage static. The authors open flat surface, based on the fact that fibers can arise during
used this equipment to successfully electrospin a PLA/gelatin electrospinning from linear clefts even without the support of a
blend, where they assessed the in situ repair of skin defects in magnetic fluid underneath.[187] The critical electric field intensity
vivo. (Ec ) required to produce fibers from free-surface electrospinning
was described as
5. Advanced Electrospinning Technologies: √
Needleless Ec = 4
4𝛾𝜌g∕𝜀20 (2)
Considering that the production output of needle-based electro-
spinning devices is commonly meager, ranging from 0.01 to 0.3 g where 𝛾 is the surface tension of the solution (N cm−1 ), 𝜌 is the
h−1 ,[184] scaling up the process has been progressively studied as density of the liquid mass (g cm−2 ), g is the gravitational acceler-
a suitable approach for industrializing this fabrication process. ation (cm s−2 ), and 𝜖 0 is the absolute permittivity (F cm−1 ). Dur-
One of the strategies that have progressed to overcome the limi- ing the onset of free-surface electrospinning, the electric force
tations of this process is the development of nozzle-less electro- is essential for Taylor cone formation and subsequent jet initia-
spinning setups. This can be achieved by scaling up the spin- tion. Prior to jet growth and the corresponding bending insta-
neret’s structure while retaining an energetically stable and well- bilities, the initial straight segment of the jets is amplified as
distributed configuration.[185] Unlike multineedle electrospin- the Coulomb forces concentrate on the leading segments that
ning, in which the electric field around a given needle is affected are trying to reach the collector.[188] The ultra-slow-motion im-
by the nearby jets, which can produce inhomogeneous fibers, ages presented in Figure 10d indicate the stages from Taylor cone
Figure 10. Roller and wire-based electrospinning. a) Diagram of a roller electrospinning setup. Modified from ref. [191]. b) Rendered CAD model of
the nozzle-free roller electrospinning setup and its variant components. Retrieved from ref. [200]. c) Schematic diagram of Taylor cone formation via
free-surface electrospinning. In the diagram, h represents the thickness of the layer, D the diameter covered by the Taylor cone, and f the electrostatic
force. Adapted from ref. [200]. d) High-speed camera depicting jet formation: i) Conical droplet on an open surface in the presence of an electric field
(time = 0 s), ii) extended conical droplet (time = 33 ms), iii) Taylor cone and jetting of the droplet (time = 66 ms), iv) depletion of the droplet (time
= 99 ms). Adapted from ref. [201]. e) Photographs depicting multijetting based on various spinneret configurations: i) roller, ii) coil, iii) disc, and iv)
wire. (i–iii) Reproduced from ref. [197]; (iv) Adapted from Nanospider (Elmarco, Ltd., Czech Republic). Copyrights: (a) Adapted with permission.[191]
Copyright 2012, Hindawi; (b, c) Reproduced with permission.[200] Copyright 2021, Elsevier. (d) Adapted with permission.[201] Copyright 2012, American
Chemical Society; (e) (i–iii) Reproduced with permission.[197] Copyright 2012, Taylor & Francis; (d) (iv) Reproduced from Elmarco, Ltd.
formation to jet depletion, which occur within a tenth of a second. During roller electrospinning, a rotating cylinder electrode
The section below discusses in detail the different forms of (roller spinneret) is partially submerged in a polymer solution
needleless electrospinning equipment that have been developed. bath against a biased rotating collector electrode under constant
airflow. Two motors control the rotating speed of the spinneret
and collector cylinders. As the spinneret rotates, a fine layer of
polymer forms at the upward-facing, non-submerged surface of
5.1. Free-Surface Roller and Wire-Based Electrospinning the spinneret. A high-voltage power with a potential (generally
greater than 50 kV) is then applied between the two rotating elec-
Roller electrospinning is the first described needleless method trodes, inducing the formation of multiple Taylor cones emerg-
capable of continuous fiber production. This method was in- ing from the surface of the rotating electrode immersed in the so-
vented by Jirsak et al., who first applied for a patent application in lution bath.[189,190] When sufficient voltage is applied to the roller
2004 (application granted in 2009, US7585437B2).[24] Needleless spinneret, the liquid layer electrifies, including multiple Taylor
roller electrospinning setups consist of a roller-spinneret elec- cones to formulate along the surface of the spinneret. When the
trode, a grounded or oppositely-charged rotating collector, a so- voltage reaches a critical value, multiple jets stretch from numer-
lution tank, a motor, and a high-voltage power supply (Figure 10 ous locations to form fibers in an upward motion on a large scale.
and Table 11). Under a strong electric field, the jets are directed and deposited
Table 11. Advantages and disadvantages of free-surface roller and wire-based electrospinning.
1. Free-surface electrospinning based on the described configurations can 1. The fiber diameters produced are usually larger than those produced by
attain high production rates through a continuous process, making it a viable conventional electrospinning, while the process requires higher voltage for
approach for industrial production.[ 202] jetting.[ 191]
2. Increasing the polymer concentration increases productivity based on the 2. Low controllability. Optimizing the parameters for consistency is much more
weight of dry fibers collected.[ 203] Increasing the conductivity of the polymer complex than conventional electrospinning, primarily due to free-surface
solution will have a direct effect on the number of Taylor cones forming, and electrospinning being guided by random Taylor cone organization through
thus the incorporation of salts as additives is a common practice of further the openly exposed polymer surface rather than a well-controlled individual
increasing fiber output. Taylor cone in the case of needle-based electrospinning.[ 202] This, in most
instances, is associated with much higher solvent and polymer wastage.
Further optimization of the process should focus on reducing the proportion
of un-spun polymer solution during the process.
3. Higher fiber production can be achieved while bypassing issues associated 3. Difficulties obtaining consistent fibers and advanced fiber configurations,
with nozzle-based setups, such as clogging and neighboring needle jet such as multicomponent composite structures. This is primarily due to the
repulsion and deviation. simple design of the spinneret and problems associated with solvent
evaporation, and more strict solution requirements for successful
electrospinning.[ 203]
on the collector’s surface, which is placed at a fixed distance from onto a mechanical energy harvester, obtaining a higher instanta-
the spinneret. Because of this, the roller electrospinning method neous output power than similar state-of-the-art devices.[199]
is a continuous and efficient process for fabricating NFs.[191] Be- Although roller electrospinning presents a high-volume out-
sides fluctuations in the conductivity of the polymer solution,[192] put and is easy to operate once the appropriate solution and elec-
variations in the shape of the spinneret play a vital role in the mor- trospinning parameters have been established, it can be challeng-
phology and diameter of the formed fibers.[193–196] ing to maintain consistent solution concentration and viscosity.
Generally, variations of the first described roller electrospin- Furthermore, due to the high electric force, incomplete solidifi-
ning method differ in the architecture and geometry of the free- cation of the fibers can allow residual solvents to be incorporated
surface spinneret. Within the roller electrospinning derivation, a into the scaffolds, which may affect the biocompatibility of the re-
roller can be in the shape of a cylinder, disc, or ball.[197] To bet- sulting constructs; nevertheless, postfabrication treatments may
ter control the energy distribution, polymer layer thickness, and resolve this issue in most cases. In addition, a major concern is
solvent exposure time, which are essential to obtain morpholog- that as the polymer solution is openly exposed to ambient con-
ically consistent fibers, spinnerets of wire and spiral configura- ditions, highly volatile solvents may rapidly evaporate, leading to
tions have been designed.[45] These were inspired by work con- fluctuations in the conductivity and viscosity that can negatively
ducted by Zhou et al. in 2014 that designed a spinneret consisting affect fiber uniformity and the consistency between experiments.
of two metal wires aligned parallel and near each other, capable This can be partially regulated by restraining the exposure of the
of formulating compound Taylor cones out of polyacrylonitrile polymer solution in the open air, the solvent system selection,
(PAN)/isophorone diisocyanate (IPDI), ultimately producing the regulating the ambient conditions, and the configuration of the
first core/shell nozzle-less electrospun fibers at a high production spinneret (e.g., using a double-motion cartilage system to deposit
rate.[198] At present, Nanospider (Elmarco, Ltd., Czech Republic) the polymer solution and take up the excess polymer on the way
has developed a commercially available industrial-scale electro- back). Thus, it is necessary to accurately tune all solution, electro-
spinning device based upon this concept, where a high-voltage spinning, and ambient parameters to achieve a consistent fiber
potential (up to 80 kV) facilitates the formation of fibers out of a production output.
polymer-layered thread at a defined rate. In recent years, the de-
vice has seen great commercial success through its production
lines, Infinity and Linea, with research groups using it to report 5.2. Bubble Electrospinning
high-throughput fiber production.
Recent developments of free-surface apparatuses have suc- Liu et al. invented bubble electrospinning in 2007.[39] As the
cessfully managed to produce binary and trinary composite fibers name suggests, this innovative method facilitates free-surface jet-
incorporating synthetic (PVP, polyglycerol sebacate [PGS], and ting, out of an open polymer surface, by gassing a polymer solu-
PCL) and naturally derived (silk fibroin) polymers that presented tion, causing it to form polymer bubbles near the surface. The
improved surface chemistry, good adherence, and proliferation of spontaneous formation of bubbles on the liquid surface reduces
fibroblasts in vitro and superior mechanical properties for skin the surface tension of the electrospinnable solution, making it ad-
tissue engineering applications. Earlier this year, a roller elec- vantageous to other free-surface electrospinning configurations.
trospinning setup was used to produce 3D electrospun PVDF Liu et al. showed that the process could yield ultrafine NFs at a
polyvinylidene fluoride-co-trifluoroethylene (PVDF-TrFE) fibers 7.5 g h−1 production rate out of a single bubble by applying volt-
presenting superior intrinsically enhanced piezoelectric proper- age ranging from 16 to 35 kV.[39] Figure 11 illustrates a typical
ties through the integration of high-throughput produced NFs bubble electrospinning setup consisting of a solution reservoir
Figure 11. Bubble electrospinning. a) Schematic diagram of bubble electrospinning apparatus. b) A proposed method of producing core/shell NFs via
co-axial bubble electrospinning; i) schematic of the process; ii) schematic of the mechanism depicting hybrid polymer bubbles forming at the surface
between the two individual polymer solutions at the interface; iii) TEM image of the attained core/shell PVA and nylon-6 hybrid fiber structure. Adapted
from ref. [204]. Adapted with permission.[204] Copyright 2021, Springer Nature.
Table 12. Advantages and disadvantages of bubble electrospinning.
1. It can be used for the mass production of NFs and scaled up for industrial 1. The constant evaporation of large amounts of solvent from the open surface
applications.[ 39 ] This has been demonstrated by SNC Fibers (Stellenbosch, area makes the process less safe for the operator and less environmentally
South Africa), which have employed bubble electrospinning for commercial friendly when harmful organic solvents are used for production.
production.
2. Breakage of large bubbles and subsequent formation of daughter bubble 2. The process is more susceptible to ambient conditions, with parameters
cascades lowers the surface tension that must be overcome for Taylor cone surrounding the viscosity of the polymer solution and solvent volatility, rate
formation, thus requiring lower working voltages compared to other of bubble formation (gas input), and electrospinning parameters requiring to
high-throughput methods.[ 211] remain at consistent levels to obtain homogenous reproducible fibers. These
factors are affected by the pressure difference between the bubbles that have
not reached the surface, and the external environment, which directs the
surface tension of the bubbles.[ 39 ]
with a submerged gas tube and a metal electrode fixed at the bot- The mechanism is driven by a surface-induced force and geo-
tom of the reservoir, a gas pump, a high-voltage power supply, metrical potential. The authors theoretically and experimentally
and a collector plate (Table 12). described that polymers mixed in a semi-solid state during the
Initially, the reservoir is filled with the polymer solution. Gas process could form an interface in a single fiber strand.[204] This
pushed from the bottom of the polymer liquid generates bubbles exciting approach will require further characterization and opti-
at the reservoir’s surface. This will incite air bubbles of assorted mization to facilitate the consistent production of core/shell NFs
sizes to emerge from the bottom of the reservoir and rise to the via this process rather than only a proportion of those present in
surface of the aerated working solution. An electric field is ap- the interface.
plied by wiring the solution with high voltage, causing the menis- Among the several variations of open liquid electrospinning
cus bubble to rupture.[204] Upon rupture, microscopic charged technologies, Korkjas et al.[99] recently developed a needleless
droplets form at the surface, which due to electrostatic repul- ultrasound-enhanced electrospinning technique (USES) to gen-
sion, become finer in size and break into smaller bubbles. The erate multilayered nanofibrous membranes. USES generates
force induced by the surface is much greater at a smaller bubble an acoustic fountain by applying a high-intensity ultrasound
radius.[204] Once the critical surface tension is overcome, the mi- to an electrified polymer solution instead of a gassing, de-
crobubbles at the solution’s surface become unsteady, formulat- positing fibers in an upward motion. In this work, the con-
ing individual Taylor cones. Once the electrical force overcomes ventional electrospinning parameters, along with the frequency
the surface tension, a jet will be discharged from the conically and amplitude of the ultrasound signal generator, were ap-
shaped microbubble toward the grounded collector. propriately adjusted to formulate bilayered PEO nanofibrous
During bubble electrospinning, bubble collapse and wrinkle mats.
of the liquid sheet are responsible for Taylor cone formation and
jetting.[205] Based on work by Oratis et al.[206] on bubble collapse
dynamics that mathematically showed that surface tension drives 5.3. Corona Electrospinning
bubble collapse and initiates wrinkle formation, earlier this year,
He et al. used this principle to evaluate the maximal wrinkle angle Corona electrospinning is an advanced high-throughput needle-
for bubble electrospinning at 49°–50°.[207] It is worth mentioning less electrospinning method patented by Molnár, Nagy, Marosi,
that the threshold voltage needed to overcome surface tension is and Meszaros in 2012.[202] Corona has benefits over other needle-
influenced by the size of the bubbles and the gas pressure inside less apparatuses as the process works without an open liquid
them. surface, with the solution flowing continuously through the
Bubble electrospinning has been successfully employed to unique architecture of the spinneret, significantly reducing prob-
electrospin a range of synthetic polymers. Li et al. have fab- lems associated with solution exposure. The setup consists of a
ricated polymer blends of PVA, PVP, and PAN incorporat- corona spinneret, a high-voltage power supply, a circular elec-
ing ZrCl2 to produce high-temperature-resistant adsorption and trode with a sharp edge, a grounded collector, and a feed sup-
separation membranes.[208] Liu et al. successfully produced ply unit. A schematic drawing of the procedure is depicted in
PVDF/FeCl3 ·6H2 O composite NFs, which were subsequently cal- Figure 12 (Table 13).
cinated to create 𝛼-Fe2 O3 NFs for catalysis.[209] Toward naturally The main working principle of this setup is to allow jets to
derived polymers, Zhao et al. successfully electrospun silk fi- generate from the edges of the circular electrode. The feed pump
broin/chitosan blends via bubble electrospinning.[210] Recently, delivers the working fluid from the bottom to the top of the spin-
Ali et al.[204] described the production of core/shell NFs via co- neret, and the polymer solution is continuously fed through a
axial bubble electrospinning. The authors illustrated that it is fea- long, narrow gutter bound to a metallic electrode with sharp
sible to attain composite core–sheath NF architecture via bubble edges. Due to the rotating spinneret, the liquid is evenly dis-
electrospinning by incorporating two polymer reservoirs in a par- persed and homogeneously distributed toward the edge of the
allel configuration, as shown in Figure 11b, thus producing sin- circular electrode, forming cones and jets along the circular gut-
gle polymer and hybrid fibers at the surface during the process. ter. The sharp edge of the electrode contains the highest electrical
Figure 12. Corona electrospinning. a) Schematic diagram depicting the corona electrospinning process, with (1) high-voltage power supply, (2) circular
electrode having a sharp edge, (3) grounded collector screen, (4) fiber formation space, (5) lid, (6) solution feed, and (7) traction of the collector
textile. Reproduced from ref. [202]. b) CAD depicting the design concept of the spinneret. c) Schematic drawing of the C-ACES method coupled with AC
high voltage. Reproduced from ref. [212]. d) Photograph indicating multiple Taylor cone formations along the edges of the 100 mm diameter spinneret.
Reproduced from ref. [46]. Copyrights: (a, b) Reproduced from patent;[202] (c) Reproduced with permission.[212] Copyright 2019, Elsevier; (d) Reproduced
with permission.[46] Copyright 2016, Elsevier.
Table 13. Advantages and disadvantages of corona electrospinning.
1. As it combines a nozzle-free spinneret configuration where fibers can be 1. To achieve high-throughput production,it is essential to rotate the spinneret
generated from its edges while the polymer solution is continuously fed into at a certain speed to prevent overflowing and to match the flow rate of the
the system at a high flow rate, high-throughput production is achievable.[ 202] polymer solution with the rotation speed of the spinneret.[ 46]
2. As the method does not constantly expose the polymer solution to an open 2. The process requires extremely high voltage (as high as 100 kV), which can
surface, this method does not have an open liquid surface; it minimizes increase the puchasing and operating costs of the power supplies and make
morphological inconsistencies due to solvent evaporation affecting the the process less safe for the operator.[ 212]
electrospinning process parameters. Therefore, it is possible to use volatile
and low boiling point solvents to fabricate NFs, making it an especially
interesting approach to producing NFs for pharmaceutical use.[ 46 ]
3. The process can be more economical since there is minimal wastage; the 3. The process has not been extensively studied or replicated by other groups,
entirety of the polymer solution added to the system can be electrospun. In with only four papers reporting the use of this technology on Scopus
contract, in free-surface setups, whatever is not electrospun must be (Elsevier’s abstract and citation database). Further research is required to
discarded due to the exposure to ambient conditions.[ 46 ] optimize and reduce some processibility parameters (such as the high
voltage) and to attempt to produce more intricate structures.
charge density, promoting the formation of Taylor cones, which Recent work by Farkas et al.[212] has managed to further in-
allows many Taylor cones to self-assemble at the sharp edges of crease the production rate of the process, reaching 1200 mL h−1
the spinneret simultaneously. When the electric field strength in- via corona alternating current electrospinning (C-ACES), a varia-
creases, multiple jets will eject from the tip of the Taylor cones. tion of corona that combines the intense forces of an alternating
After solvent evaporation, fibers are collected in an upward mo- electrostatic field with corona’s sharp-edged spinneret configu-
tion. The initial prototype design of the spinneret reached pro- ration. The approach is conceptually similar to corona but uses
duction rates up to 300 mL h−1 .[46] an alternating current power supply rather than direct current
Figure 13. High-speed electrospinning. a) Schematic diagram of the high-speed electrospinning method. b) Photograph of the device with a continuous
cyclone sample collector. Reproduced from ref. [213]. SEM images of c) 𝛽-galactosidase containing 2-hydroxypropyl-beta-cyclodextrin-based fibers and d)
Kollidon VA 64 loaded with itraconazole. Reproduced from refs. [213] and [49] , respectively. Copyrights: (a, b) Reproduced with permission.[213] Copyright
2015, Elsevier; (c, d) Reproduced with permission.[49] Copyright 2020, Elsevier.
Table 14. Advantages and disadvantages of high-speed electrospinning.
1. Capable of continuous production of large quantities of fibers at a fiber 1. This process cannot produce complex structures (e.g., core–shell).
output of 450 g h−1 .
2. As the process does not present a free liquid surface, it can be used with 2. The process requires an extremely high rotational speed and high voltage.
volatile and low boiling point solvents, similar to corona electrospinning. The fibers produced via this process present secondary morphologies (e.g.,
beads) and lack homogeneity with a large standard deviation in fiber
diameter.
3. Fibers are collected in a cyclone rather than a collector, a new approach that 3. More research is required to evaluate this relatively new process’s advantages
can produce fragmented fibers, which helps their downstream processing for and limitations and better understand the processing parameters.
pharmaceutical applications.
high voltage. During electrospinning, the authors used an annu- The setup (Figure 13 and Table 14) consists of a stainless-
lar orifice spinneret 110 nm in diameter, rotating at 100 rpm, ap- steel disc-shaped spinneret equipped with 36 equidistantly dis-
plying a 100 kV voltage at a 50 Hz frequency at a feeding rate tributed orifices on the wheel’s side wall. The spinneret rotates
ranging from 100 to 1200 mL h−1 , collecting fibers in an upward via a high-speed motor. The rotational speed of the spinneret can
motion from a 75 cm distance (between the spinneret and the be increased up to 50 000 rpm. This high-speed rotation exerts
collector’s surface). The authors employed this technique to pro- a centrifugal force on the solution, which is forced through the
duce PVP K90 NFs loaded with spironolactone (an aldosterone orifices of the spinneret, allowing the jet formation to occur in
receptor antagonist).[212] the presence of a high voltage (greater than 40 kV). The fibers
are collected within a cyclone rather than a collector surface af-
ter jetting. This way, no free liquid surface is present, and sol-
5.4. High-Speed Electrospinning
vent evaporation from the solution is minimized before fiber
formation starts, which helps maintain the solution’s concen-
In 2015, Nagy et al. first described high-speed electrospinning to
tration and viscosity during the electrospinning process. Using
produce co-polyvidone (Kollidon VA 64) NFs loaded with a poorly
this method, the authors evaluated the production rate at ≈450 g
water-soluble antifungal drug, itraconazole.[49] High-speed elec-
h−1 (at a feeding rate of 1500 mL h−1 ), with the possibility of
trospinning combines electrostatic and high-speed rotational jet
each electrospinning reactor producing about 10.8 kg d−1 .[213]
generation and fiber elongation resulting in a significant increase
Such a scaled-up, continuous, flexible manufacturing process
in fiber production output.[213]
can meet the capacity requirements of the pharmaceutical nificant amounts of solvent needed for electrospinning and their
industry. negative environmental and health impact.
Co-axial and multi-axial electrospinning present similar lim-
itations. The principal constraint of the process is that all the
6. Comparison of Different Methods polymer solutions used must be compatible; otherwise, electri-
cal forces cannot draw them together without coagulation. To en-
Table 15 comparatively summarizes the key advantages and dis-
sure the development of a compound Taylor cone at the tip of
advantages of the different electrospinning techniques.
the spinneret, it is essential to maintain its concentric structure
throughout the jet expansion and for the entire process duration.
7. Discussion and Limitations The second limiting factor is that each solution must present
similar physicochemical properties. A suitable viscous force is
Despite the apparent advantages and broader applicability of elec- needed to maintain the Taylor cone and prevent its separation
trospun fibers over other fiber preparation techniques, as shown during the bending instabilities stages of jetting. This is a valid
in Table 15 above, each and every one of the electrospinning concern when one of the solutions dries faster than the other.
methods described in this review carries its limitations. When the working solutions are compatible, the co-axial and tri-
The most recognized limitation of conventional electrospin- axial electrospinning methods tend to be successful upon appro-
ning is the low production rate and the fact that not all mate- priate parametric assessment. The third limiting factor is the bal-
rials are appropriate for electrospinning. For example, because ance between the flow rates of different solutions. Variations in
of their low molecular weights, many conductive polymers have the flow rate will affect the final compound fiber quality. A low
relatively low solubility in commonly used solvents. They lack flow rate would disrupt fiber formation, while a high flow rate
enough chain entanglement to maintain stability. Additionally, would break the structure. Finally, the fourth limiting factor is
due to their highly conductive nature, forming a steady jet is chal- the design of the complicated concentric spinneret, which plays
lenging. Therefore, electrospinning them into fibers is challeng- an essential role in this method. The spinneret provides a suitable
ing. A commonly used approach is mixing them with other elec- working environment for attaining NF of the desired configura-
trospinnable polymers. However, in this instance, the compati- tion, and it can positively or negatively influence the composite
bility of the two materials should be taken into consideration. droplet’s behavior under the electric field.
When it comes to tissue engineering, one of the main concerns 3D electrospinning is the only reported technology capable
with conventional electrospinning is the limited cell infiltration of producing 3D microstructures in the micro/nanoscale in a
into the electrospun scaffolds and restricted tissue ingrowth due single-step process—3D electrospinning benefits from unifying
to their highly dense 2D structure and small diameter pores. The a fused deposition modeling 3D printing architecture with elec-
compact and superficial porous structures of these scaffolds re- trospinning. The technology has been successfully employed to
sult in low cell penetration. The high porosity and small pore size produce woven electrospun structures by directing the deposition
associated with conventional electrospun fibers are directed by of the fibers via a Cartesian coordinate system. As a relatively new
the diameter of the fibers and fiber interconnectivity. This phe- fabrication approach, research should focus on building more
nomenon becomes more pronounced as the diameter of the NFs mechanically stable structures. Although cryo-electrospinning
decreases. While the inherently porous structure of electrospun and wet electrospinning can produce non-woven randomly ori-
scaffolds provides fenestrations that are insufficient for most cell ented 3D structures, both processes are limited to the availability
types to pass through, they are sufficient for nutrient and cytokine of compatible polymer–solvent systems and, in most instances,
transport. Whilst cellular expansion in the form of a monolayer is require post-fabrication processing to obtain the final 3D form.
not problematic for the development of wound dressings, as the Portable electrospinning is a fascinating technology that illus-
construct is merely meant to facilitate cell migration and prolifer- trates the feasibility of electrospinning using a battery-powered
ation, 3D structures can further enhance fluid retention and ex- handheld apparatus, producing NFs at a lower voltage in an in
udate absorption. Further research in post-fabrication technolo- situ manner. This technology has potential in wound healing
gies such as freeze-drying and gas-foaming to expand the scaf- management, as it allows for the direct deposition of fine fibrous
fold’s 2D structure or advancements in technologies such as 3D layers in open wounds, which can protect the wound bed from in-
electrospinning can, in due course, resolve these issues. fection and promote healing while reducing patient discomfort.
The possibility of residual toxic chemicals remaining within Although the process has been successfully used to incorporate
electrospun fibers is another limiting factor. The properties of pharmaceutical compounds into a range of synthetic polymers
the selected solvent are a critical electrospinning parameter, as and a clinical trial assessing the effect of portable electrospin-
it can determine whether a specific polymer can be electrospun ning in wound healing is ongoing, further research is needed
and directly affect the morphology of the produced fibers . Highly to address operational safety concerns, solvent limitations (due
volatile solvents are generally used in electrospinning to produce to residual solvents) and the stability of the process toward fiber
dry fibers. However, in a some cases, residuals remain on the morphology.
surface of the electrospun fibers, which could lead in cytotoxicity The primary limitation of the needleless electrospinning tech-
when the fibers are used in medical and pharmaceutical applica- niques is mainly related to the relatively sizeable free liquid sur-
tions. Moreover, many postprocessing procedures rely on harsh face exposure during the process. Bubble electrospinning, in par-
substances that can pass through to the final product. The use ticular, has immense free liquid surface exposure due to bub-
of organic solvents for electrospinning requires further investi- bling. Alongside the formation of polymer jets, solvent evapo-
gation into the use of green solvents when considering the sig- ration can be detrimental to the surrounding environment and
Table 15. Comparison of different methods based on the advantages and disadvantages.
Electrospinning Advantages Disadvantages

technique
Needle-based Mono-axial 1) Well-studied, simple setup, easy to operate. 1) Low productivity.

2) An easy way to evaluate the electrospinnability of new 2) Simple fiber architecture (monolithic).
materials and optimize parameters. 3) Single fiber configuration.
3) Morphologically consistent NFs can be produced. 4) Compact 2D structure of high density and small pore size.
4) Composite fibers can be developed via blending.
Co-axial 1) Creates novel core–shell or hollow structures. 1) Low productivity.
2) Tune (drug) release profiles. 2) Relatively complicated spinneret.
3) Can produce NFs from otherwise unspinnable materials. 3) Difficult to implement and balance the flow rates of
different fluids in a composite jet.
Tri-axial 1) Creates a novel trilayer structure. 1) Low productivity.
2) Can produce composite fibers of enhanced mechanical 2) Complicated spinneret structure.
stability and biocompatibility (e.g., incorporating synthetic 3) Difficult to implement and balance the flow rates of
polymers in the multiple cores and naturally derived different fluids in a composite jet.
material in the sheath). 4) Arduous and time-consuming process of cleaning the
3) Can produce complex drug-release systems. spinneret. Taylor cone stability requires constant
4) Can produce NFs from unspinnable materials. supervision.
Centrifugal 1) Can obtain homogenous NFs of variant diameters. 1) A relatively new method that requires further investigation
2) Produces loosely packed microfibrous structures that can of the parameters influencing the process.
enable better cell infiltration. 2) Single fibers with simple structure. Only a few recent papers
3) Combines the advantages of traditional electrospinning and have focused on attaining core/shell fibers.
centrifugal spinning techniques. 3) Nozzle clogging and unconventional collector
4) Can be scaled up. configurations.
3D 1) The only single-step method capable of producing 3D 1) Relatively new method.
fibrous structures. 2) Polymer systems with higher conductivity are necessary for
2) Woven or nonwoven structures are obtainable with 3D assembly.
processes such as 3D electrospinning or 3) Increasing the height of the 3D structure reduces the
cryo-electrospinning, respectively. precision of the process.
3) The shape and macromorphology of the 3D structure can 4) Poor mechanical stability.
be directed.
Portable 1) The only method capable of in situ electrospinning. 1) Extremely new technology.
2) Mostly applicable for wound healing, with the potential of 2) Poor stability during electrospinning and safety concerns
being used for on-site wound management. (e.g., residual solvents).
3) Cordless, handled electrospinning setup powered by a 3) Predominately used with water and ethanol-soluble
battery. polymers; issues associated with solvent evaporation need
4) Can incorporate pharmaceutical compounds or other active to be addressed.
substances and nanomaterials (e.g., nanoparticles).
Needleless Roller 1) High-throughput production of micro/nanostructured 1) Predominately produces large fiber diameters of a high
fibers. standard deviation and less morphologically consistent
2) Continuous fabrication can be implemnted for fibers than needle-based setups.
industrial-level production. 2) Requires a higher voltage to initiate jetting compared to
3) Easy to manipulate the production rate and fiber diameter. needle-based setups.
4) The most researched needleless method in the literature. 3) Susceptible to ambient conditions; solvent volatility due to
the exposed open surface, which can affect fiber
homogeneity.
Bubble 1) High production rates are attainable; it has been 1) A newly described and not yet thoroughly researched
successfully employed for mass production. technology.
2) Can be operated with a low voltage compared to other 2) The large exposed area poses safety issues for the operator
needleless methods. and environment when toxic solvents are used.
3) Susceptible to ambient conditions and air pressure, reduces
fiber homogeneity when electrospinning is prolongated.
Corona 1) Low-free liquid surface spinneret. 1) Requires a certain rotating speed to avoid overflow.
2) Continuous high-throughput fabrication is feasible. 2) Requires extremely high voltage.
3) Unique spinneret architecture allows polymer solution 3) A relatively new process needing further research to
shielding while instantaneously promoting high-throughput understand its advantages and limitations.
electrospinning.
High-speed 1) High productivity (≈0.5 kg h−1 ). 1) Production of complex fiber structures (core–shell) is not
2) Continuous fiber production is possible. possible.
3) Fiber fragmentation in the collector cyclone can help 2) Process requires extremely high rotational speed and high
downstream processing. voltage.
3) A relatively new process requiring further research to
understand its advantages and limitations.
harmful to the operator. In extreme cases, when the concentra- ing environment. This is not ideal for the mass production of
tion of the combustible solvent accumulates to a critical value, it fibers in the industry. Although a significant amount of work
will cause ignition. Another concern is that a large liquid surface has been carried out using aqueous polymeric solutions as a
enhances water absorption from the air, diluting the spinning less harsh alternative to organic solvents, when the processibil-
solutions and thus affecting fiber consistency and quality. In ad- ity of the polymer in water is not feasible, directing the focus
dition, needleless electrospinning technologies are overall asso- toward the use of “green” solvents is essential. Although using
ciated with poorer fiber homogeneity and reduced consistency melt electrospinning seems like a simple approach to meet these
among batches. The higher critical potential required to attain requirements, the process has limitations concerning the com-
Taylor cone formation in needleless electrospinning methods of- plexity of the fibers produced, producing fibers large in diameter,
ten limits the selection of polymers that can be electrospun, and polymer-related thermal degradation, and incompatibility with
the complexity of the polymer system. Thus, these techniques several high-throughput technologies discussed in this review.
have limitations in polymer selection, operating costs, and en-
vironmental concerns. Additionally, it will be a long time be-
fore needleless electrospinning methods can fabricate NFs with 9. Conclusion
complex structures such as side-by-side and core–sheath cross- It is universally acknowledged that electrospinning has played a
section configurations. significant role over the past two decades in developing diverse
Many approaches have been considered to overcome the prob- advanced nanostructured materials for almost every conceivable
lems associated with fiber quality and reproducibility when us- application. Researchers from around the globe have contributed
ing needleless setups. First, needleless setups can be enclosed in to the evolution of the electrospinning principles, uncovering the
sealed transparent containers to reduce solvent evaporation. The process’s capabilities and discovering technologies and methods
humidity inside the container can be controlled to prevent sig- to move forward and push the limits of this technology. Signifi-
nificant water absorption from the air. Second, by modifying the cant progress has been made in understanding its principles and
design of the spinneret and optimizing process parameters, the exploring its applications, as has been documented by the expo-
ejecting speed and jetting can be accurately manipulated. Finally, nential and consistent increase in the number of publications
developing spinneret configurations that limit polymer exposure and patents filled in the past two decades.
while retaining a high surface electrode area for high-throughput This review focused on comparing the advantages and limi-
production is an effective way of improving consistency. tations of needle-based and needleless electrospinning technolo-
gies. A brief history and background knowledge of the electro-
8. Future Perspectives spinning principles were highlighted. Generally, the fundamen-
tal problem associated with needle-based techniques is scaling
Although it is easy to recognize that electrospinning is a fascinat- up limitations and operational complexities. For needleless pro-
ing technique for fabricating a large variety of intriguing micro cesses, on the other hand, the critical issues are related to the
and nanoscaled materials, potential problems still need to be ad- large free liquid surface, which results in economic and environ-
dressed. mental issues and difficulties in obtaining morphologically con-
A small proportion of the research has focused on modeling; sistent batches between experiments. Many parameters of newly
however, a universally accepted simulation model for accurately invented techniques still need to be optimized.
predicting the needle-based or needleless electrospinning param- The future of each technology and its advancement or dis-
eters has not yet been developed. As a result, the majority of elec- missal will depend on specific application requirements, includ-
trospinning experiments rely on an empirical understanding of ing specialized structures, multifunctional hierarchical organi-
the process requirements and parametric studies. For instance, zations, and scaling for industrial production. The combination
in needleless electrospinning, the challenge remains in produc- of electrospinning with other fabrication methods (e.g., bioprint-
ing uniform fibers with high output while simultaneously obtaining) holds a promising future for numerous applications.
ing the desired fiber diameter, structure, and application-specific
properties . To overcome these limitations, researchers should be
more open to sharing positive and negative results on optimizing Acknowledgements
the different parameters of the techniques, including solution, For the purpose of open access, the authors have applied a Creative Com-
process, and ambient conditions. This approach will help to bet- mons Attribution (CC BY) license to any Author Accepted Manuscript
ter understand and control the morphology and reproducibility of version arising from this submission. Short sections of this review were
each technology. This progress will help better predict the Taylor adapted from the first author’s doctoral thesis. A.K. and N.R. would like to
cone formation requirements, jet behavior, and fiber output. acknowledge the late Dr. Giuseppino Fortunato for his outstanding contri-
Another critical concern is the economic and environmental butions and expertise in the field.
aspects of the processes. Over the years, many solvents have been
successfully used to produce electrospun fibers through solu- Conflict of Interest
tion electrospinning. However, the predominant number of sol-
vents used to formulate fibers today can significantly impact the The authors declare no conflicts of interest.
environment and human health by being harmful to humans
and ecosystems. This is especially true for needleless electro-
spinning since it has a large liquid surface exposed to the air,
Keywords
and highly volatile solvents are evaporated into the surround- 3D electrospinning, advanced fibers, corona, electrospinning, needleless
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Antonios Keirouz is currently a postdoctoral research associate at the University of Bath working on
developing advanced minimally and noninvasive biosensing interfaces. He holds a Ph.D. from the
University of Edinburgh in collaboration with the Swiss Federal Laboratories for Material Science and
Technology (Empa), an ETH Domain institute. Dr. Keirouz has worked closely with scientists, engi-
neers, and clinicians on a wide range of projects surrounding skin tissue engineering, drug-eluting
biomaterials, and biosensors, with a profound interest in electrospinning.
Seeram Ramakrishna, FREng, Everest Chair is a world-renowned poly-disciplinary scholar at the Na-
tional University of Singapore. He is named among the World’s Most Influential Minds (Thomson
Reuters); Top 1% Highly Cited Researchers in material science as well as cross-field categories (Clar-
ivate Analytics); and World Top 100 Scientists 2023. His publications to date have an H-index of 177
and over 153 637 citations. He is an elected fellow of UK Royal Academy of Engineering, AAAS, ASM
International, ASME, and AIMBE, USA. He is an editorial board member of RSC Energy and Environ-
mental Science, NPJ Urban Sustainability, eScience, and Advanced Fiber Materials.
Norbert Radacsi is a senior lecturer in chemical engineering and director of the NanoMaterials Labo-
ratory at The University of Edinburgh. He obtained his Ph.D. at the Delft University of Technology. Prior
to his current position he was postdoctoral researcher at Purdue University and California Institute of
Technology. He has pioneered a new type of 3D electrospinning technology. His interdisciplinary re-
search includes areas of advancing electrospinning technology and bioprinting, developing wearable
sensors and energy harvesters, and producing novel materials.

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REVIEW

The History of Electrospinning: Past, Present, and Future

nanoﬁbers (NFs), and the ease of manip-

A. Keirouz, Z. Wang, N. Radacsi A. Keirouz

Parameters Inﬂuence on electrospinning

Parameters Inﬂuence on electrospinning

Solvent system Polymer (additives) Electrospinning technique Ref.

2-Methyltetrahydrofuran (2MeTHF)/formic Poly(3-hydroxybutyrate-co-3-hydroxyvalerate Mono-axial (using a syringe heater, to [87]

The electrospinning techniques introduced in this review are

Table 5. Advantages and disadvantages of mono-axial electrospinning.

Table 6. Advantages and disadvantages of co-axial electrospinning.

Table 7. Advantages and disadvantages of tri-axial electrospinning.

Table 8. Advantages and disadvantages of centrifugal electrospinning.

Table 9. Advantages and disadvantages of 3D electrospinning.

Table 10. Advantages and disadvantages of portable electrospinning.

Table 12. Advantages and disadvantages of bubble electrospinning.

Table 13. Advantages and disadvantages of corona electrospinning.

Table 14. Advantages and disadvantages of high-speed electrospinning.

Electrospinning Advantages Disadvantages

Needle-based Mono-axial 1) Well-studied, simple setup, easy to operate. 1) Low productivity.

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