7

Nano-Fibres for Filter Materials

K. Schaefer, H. Thomas, P. Dalton, and M. Moeller

Summary. Textile materials are used for a variety of dry and wet filtration
processes allowing either the increase of the purity of the material filtered or the
recovery of solid particles. Typical examples for textile-based filtration processes
are air filtration, process filtration (e.g. solid–liquid separation), industrial effluent
treatment or dehydration of sewage sludges.
Current conventional textile filters consist of natural or human-made fibres with
diameters ranging from a few single to a few ten microns. Small fibres are well
known to provide better filter efficiency which is related to the increase in surface-
area-to-weight ratio. For this reason, nano-fibre filter media enable new levels of
filtration performance for several applications in different environments ranging from
industrial and consumer to defence filtration processes.
Nano-fibres with diameters between 100 nm and 3 µm are readily accessible by
the electrospinning process. Electrospinning uses a high electrical field to draw a
polymer solution (or melt) from the tip of a capillary to a collector. By applying
voltages of approximately 10–50 kV, fine jets of the solution (or melt) can be drawn
to a grounded or oppositely charged collector. The evaporating solvent (or cooling
of the melt) results in fibres that are collected and formed into nano-fibre mats with
adjustable fibre diameters mainly based upon solution viscosity and electrical field
strength.
A broad range of polymers ranging from natural and synthetic organic to inor-
ganic polymers can be electrospun from the solution or melt allowing the genera-
tion of tailored nano-fibre webs for various applications. Furthermore, the nano-fibre
webs may be used as carrier material for subsequent fixation of various substances to
fibre surfaces as well as for their direct implementation into the fibre. This increases
the possibilities for production of, e.g. hygienic functionalised filters or of temper-
ature stable filters with catalytic activity. Hygienic filters produced from cationic
polymers or with incorporated silver can reduce the contamination of air or water
filters with bacteria while temperature stable filters, which can be obtained from
SiO2 -precursor or silica hybrid materials and which are loaded with metal/metal
oxide nano-particles, are destined for air pollution control.
126 K. Schaefer et al.

7.1 Introduction

Raw materials for non-wovens are generally natural or human-made fibres

with diameters ranging from about 3 to 50 µm. New levels of performance can
be enabled by nano-scaled fibres in all fields of application demanding a high
surface-area-to-weight ratio, e.g. filtration and catalysis.
Nano-fibres with diameters between 100 nm and 3 µm can be made by the
electrospinning process. The technique of electrospinning has been known from
the work of Formhals [1] since 1934 but received relatively little attention until
recently. In 1971, Baumgarten [2] performed studies on the electrospinning of
acrylic micro-fibres; he obtained fibres with diameters of 500–1,000 nm. With
increasing interest in nano-technology and motivated by the reviving work
of Reneker’s research group electrospinning has gained exponential research
interest in the last few years (Fig. 7.1) [3–6]. Since 1990s, the research groups
of Reneker, Vancso, Greiner and Wendorff investigate the electrospinning in
detail [3–14]. During the last decade, extensive investigations on the electro-
spinning process have been conducted from different viewpoints like aspects of
theoretical simulation [15, 16], fibre formation mechanism, influencing factors
for fibre size and morphology [17] and applications [18, 19].
A wide variety of polymers (natural, synthetic, organic and inorganic poly-
mers) have been electrospun from the solution and melt phase allowing the
generation of tailored nano-fibre webs for various areas of application, e.g. fil-
tration [18], reinforcement in composite materials [7], protective clothing [21]
or biomedical uses [22–24].

Fig. 7.1. Increase in papers on the electrospinning in the last decade [20]
 7 Nano-Fibres for Filter Materials 127

7.2 Principle of Electrospinning

Electrospinning (or electrostatic spinning) uses a high-voltage electrical field

(10–50 kV) to draw a polymer solution or melt from the tip of a capillary
to a collector (Fig. 7.2). When the electric forces at the surface of a polymer
solution or melt overcome the surface tension, an electrically charged fine jet
is formed which can be drawn to a grounded or oppositely charged collector.
The evaporating solvent (or cooling of the melt) creates fibres that are col-
lected and formed into nano-fibre mats. Electrospun fibres are continuous in
length, their diameter ranges from under 3 nm to over 50 µm depending on the
electrospinning conditions. The smallest possible polymer fibre must contain
one polymer molecule [5].
The fibre diameter of fibres formed during electrospinning is influenced by:

System parameters
– Polymer properties
Molecular weight, structure and poly-dispersity of the polymer,
concentration, melting point and glass transition point
– Solution properties
Solvent, volatility, viscosity, conductivity, surface tension, pres-
ence of further additives (e.g. salts)
Process parameters
– Ambient parameters
Solution temperature, humidity, atmosphere, air velocity in the
electrospinning chamber
– Equipment parameter
Voltage, field strength, electrode distance and arrangement,
flow rate, delivery volume, needle diameter

Pressure gauge

Pump
Solution

HV
0–50 kV
Taylor cone

Ground
Electrode
substrate
Fig. 7.2. Setup for electrospinning from polymer solutions
128 K. Schaefer et al.

The formation of fibres in the electrospinning process is mainly influenced by

the following forces:
– Surface tension
– Electrical-repellent force derived from electrical charged polymer droplets
– Visco-elastic force coming from the polymer
Higher polymer concentrations typically result in larger fibre diameters, an
increase of the electrical field strength leads to a decrease of the fibre diame-
ter. The fibre diameter shall be consistent and controllable; the fibre surface
shall be defect-free or defect-controllable. However, in practical electrospin-
ning experiments often inhomogeneous fibres with defects and beads can
occur. Splitting of the jet can occur, which results in finer fibres.

Advantages of nano-fibres:
– Fibre diameter: <3 nm to >50 µm
– High surface area to volume ratio (→ high specific surface)
– High aspect (length to diameter) ratio
– High bending performance
– Flexible surface functionalities
– Ability to control pore size in non-woven fabrics
– Possibility to insert special functionality
A further advantage of electrospinning compared to conventional solvent spin-
ning is that water can be used as solvent. Water-soluble fibres have to be
cross-linked, e.g. by thermal or by chemical cross-linking [13, 20, 25].
These advantages result in great application potentials of nano-fibres
in broad fields such as separation, adsorption, filtration, catalysis, fibre-
reinforced composites, tissue engineering, wound dressings, drug delivery sys-
tems, sensors, cleaning tissues, protective textile and other [18–29].
Nano-fibres can be spun from polymer solutions or from polymer melts.
Larrondo and Manley [30–32] were the first to carry out and report on melt
electrospinning experiments. Working with PE and PP in the early 1980s,
they successfully formed fibres with diameters only as small as the tens of
microns range. Electrospinning from polymer melts has the advantage that
no solvents are needed which have to be removed by evaporation. However, the
melting temperature of the polymers is an important influencing factor for the
applicability of the procedure to produce nano-fibres. In general, nano-fibres
which are produced by melt electrospinning have a higher fineness than those
electrospun from solutions, achieving nano-dimensions by melt electrospinning
is non-trivial (Scheme 7.1).
At DWI, a working group is using melt electrospinning for the production
of nano-fibres or nano-webs for biomedical applications like scaffolds for tissue
engineering, in vitro neuron interactions with oriented electrospun fibres or
others [33–36].
 7 Nano-Fibres for Filter Materials 129

Electrospinning

from

Polymer solutions Polymer melts

Restrictive parameters Restrictive parameters
• Solubility of polymers Melting point of polymers
• Suitable solvents with Viscosity of melts
regard to viscosity, etc.
volatility, toxicity etc.
⇒ Requirements to ⇒ Requirements to the
polymers and solvents equipment to reach the
right temperature

Results in finer (nanofibres) Results in coarser

and more homogeneous (approx. 1 µm) and less
nanofibres. homogeneous nanofibres.

Scheme 7.1. Comparison of electrospinning from solutions or from polymer melts

7.2.1 Practical Electrospinning

Typical electrospinning equipment consists of three components: a high-

voltage source, a spinneret (or nozzle) and a collector (Fig. 7.2).
The polymer solution or melt is applied into a syringe (or a spinneret)
which is equipped with a piston and a stainless steel capillary serving as elec-
trode and pushed through by a pump with a defined flow rate. The spinneret
is connected with the high-voltage source and applies high voltage to the
polymer. This results in the formation of a polymer drop at the end of the
spinneret. Under higher voltage the drop changes its shape and turns into a
conic form (Taylor cone) (Figs. 7.2 and 7.3) [30–32, 37, 38]. At a defined volt-
age, the surface tension of the polymer cone at the tip of the spinneret starts
to elongate and stretch so that a charged jet is formed. The jet moves in loops
bending and whipping towards the electrode with opposite polarity or to the
grounded target (Fig. 7.3). Recent experiments demonstrate that the rapidly
whipping fluid jet is an essential mechanism of electrospinning [39, 40].
Different collection systems are known [35]. For the usually produced non-
woven mats metal plates are used as counter electrode and collection sys-
tem of the nano-fibres or nano-webs. However, for special applications further
grounded collectors were developed (Fig. 7.4) [36].
130 K. Schaefer et al.

Fig. 7.3. Schematic presentation of the electrospinning process [41]

Fig. 7.4. Different electrospinning collection systems: (a) single plate configuration,
(b) rotating drum, (c) triangular frame placed near single plate, (d) parallel dual
plate and (e) dual-grounded ring configuration [36]

7.2.2 Nano-Fibres Produced by Electrospinning

form Polymer Solutions or Melts

In Figs. 7.5–7.10, nano-non-wovens or nano-fibres which were spun from poly-

mer solutions (here: poly(vinyl alcohol) (PVA) in water or polycaprolactone
(PCL) in chloroform/ethanol – 3/1, v/v) or from polymer melts (here: a
blend of poly(ethylene oxide-block-ε-caprolactone) (PEO-PCL) and PCL)
are shown. The melt electrospinning was performed at a temperature of
85◦ C applying the rotating drum collection system (Fig. 7.4b). High volt-
ages of 30 kV were applied during the electrospinning of PCL and 17 kV for
the spinning of PVA solutions. Nano-fibres with average finenesses of about
300–600 nm were produced by electrospinning of PVA or PCL solutions, some
very fine fibres with fibre diameters of approximately 100–300 nm were found
in electrospun PCL nano-fibres. The nano-fibres which were obtained after
melt electrospinning had fibre diameters of about 1 µm.
 7 Nano-Fibres for Filter Materials 131

Fig. 7.5. Nano-non-woven obtained by melt electrospinning of a blend PEO–PCL

and PCL

20 µm 10 µm

Fig. 7.6. Nano-fibres produced by electrospinning from aqueous PVA solutions

(average fibres in the range of 300–600 nm fineness)

7.2.3 Electrospraying

Electro-driven jets of polymeric fluids undergo instabilities causing either

breaking of the jet into droplets (electrospraying) [42–44] or splitting into
finer jets resulting in the production of superfine fibres (electrospinning). Both
processes are mechanistically similar with the exception that in electrospin-
ning high molecular weight polymers and chain entanglement in more concen-
trated polymer solutions stabilise the initial jet towards spraying (Figs. 7.10
and 7.11). Electrospraying can be used for the production of multi-functional
132 K. Schaefer et al.

100 µm 10 µm

Fig. 7.7. Nano-fibres produced by electrospinning from PCL solutions (PCL chlo-
roform/ethanol solution) (average fibres in the range of 300–600 nm fineness and the
fine fibres 100–300 nm)

Fig. 7.8. Nano-fibres produced by electrospinning from melts at 85◦ C of a blend

of PEO–PCL and PCL. Collection times are 1 min (left figure) and 6 h (right fig-
ure). The average fibres are approximately 1 µm, however with long collection times,
larger fibres are observed. Such impurities are commonly observed for both melt and
solution electrospinning

Fig. 7.9. Nano-fibres electrospun from melts of a blend of PEO–PCL and PCL onto
a conventional PET non-woven
 7 Nano-Fibres for Filter Materials 133

Mainly spraying Spraying/spinning Spinning

10 µm 10 µm 10 µm

2 % PVA 4 % PVA 6 % PVA

Fig. 7.10. Electrospraying or electrospinning in dependence on the PVA concen-

tration in solution

200 µm 200 µm

10 kV 20 kV

200 µm

30 kV

Fig. 7.11. Influence of voltage on the particle size obtained during electrospraying
of a non-polymeric organic compound

materials, too. The formation of droplets in the electrospraying process is

caused by breaking up of the jet due to Rayleigh instability [45].
Functional fibre coatings can be obtained by electrospraying, whereas,
nano-fibre webs for implementation into non-wovens are produced by elec-
trospinning.
134 K. Schaefer et al.

7.3 Application of Nano-Fibres or Nano-Webs

as Filter Media
The large surface area of nano-fibre webs allows rapid adsorption of dust and
other particles from air such as micro-organisms or pollen as well as hazardous
molecules. The latter necessitates reactive sites in the polymer or catalytically
active additives allowing chemical binding or decomposition of hazardous sub-
stances, respectively. Besides fineness and resulting large specific surface area
of nano-fibre webs, their high porosity and small pore size contribute further
to their high adsorption and filtration efficiency. Pore size and porosity of
filter media are determined by the diameter of fibres used for production of
filter media. For filter media very thin webs consisting of just a few nano-fibre
diameters thickness are effective. The thickness of the nano-web can be less
than 1–5 µm [46]. While the thinness of the nano-web provides high perme-
ability to flow, the nano-web has limited mechanical properties that preclude
the use of conventional web handling and filter pleating equipment. The small
fibre diameter of nano-fibres and the thin nano-web layer result in high filter
efficiency with minimal pressure drop increases. Furthermore, nano-fibre fil-
ter media have demonstrated longer filter lifetimes than conventional filtering
materials.
The technical requirements for filters are a balancing of the three major
parameters of filter performance: filter efficiency, pressure drop and filter life-
time. An improvement in one category generally means a corresponding sac-
rifice in another category. It was shown that the proper use of nano-fibres can
provide marked improvements in both filtration efficiency and lifetime, while
having a minimal impact on pressure drop [46].
Nano-fibre webs can be applied onto various substrates, e.g. onto conven-
tional non-wovens, too. These substrates can be selected to provide appro-
priate mechanical properties to allow pleating, filter fabrication, durability in
use, and in some cases, filter cleaning [46, 47].
In the beginning of the 1980s, Freudenberg and Weinheim started to apply
the electrostatic spinning for the development of non-wovens by arrangement
of electrospun fibres between a support layer and a preliminary filter in a
sandwich-like structure [48–50].
Donaldson Company, Inc. has been using electrospinning technology to
make fine fibres for more than two decades [18,19]. Donaldson produces Ultra-
WebTM nano-fibres with sub-half-micron diameters for air filtration in com-
mercial, industrial and defence applications [46]. Nano-fibre filter media make
new levels of filtration performance possible in several transportation applica-
tions including internal combustion engines, fuel cells and cabin air filtration.
According to Luzhansky, Donaldson produces about three pounds of nylon or
over 10,000 m2 nano-fibres per day [20, 51].
Greiner and Wendorff developed together with Hollingsworth & Vose
GmbH/JC Binzer Mill, Hatzfeld/Germany, the so-called NanowebTM , i.e. a
super-filter which is produced by electrospinning of nano-fibres onto a base
 7 Nano-Fibres for Filter Materials 135

material [20]. NanowebTM can be used for air filtration, e.g. for filtering pollen
or other particles from the air [52]. The big advantage of NanowebTM is, beside
of the optimisation of the filter capacity, the absolutely negligible materials
usage.
In Liberec, the company Elmarco developed in co-operation with the
Technical University of Liberec modified electrospinning technology called
“Nano-spider” which is based on electrospinning from non-water-based poly-
mer solutions [53–55]. Elmarco presented a pilot line at INDEX 05 in
Geneva/Switzerland, to the non-woven industry [55]. The nano-fibre materi-
als of Elmarco are developed for wide use in medical, biological and technical
fields.
Apart from using synthetic polymers bearing special functionalities or spe-
cific add-ons to the spinning solution, chemical and biological functionality
can also be achieved from natural polymers accessible from waste materials.
For example the chitin-derivative chitosan is known to provide antimicrobial
effectiveness [56] or keratin fibres are known for their propensity in binding air
polluting substances by nucleophilic addition, e.g. formaldehyde [57]. This was
the basis for us to investigate natural polymers like chitosan and wool keratins
during electrospinning [25]. Keratins isolated as S -sulpho-keratins cannot only
be electrospun but also allow the reformation of cystine bridges and thus the
fibre stabilisation after reductive removal of the protection group. Chitosan-
bearing nano-fibres or nano-fibres post-coated with chitosan can reduce micro-
bial growth and are potentially interesting for air filtration uses [25]. Fibre
formation with lower molecular weight proteins as well as chitosan needs the
addition of interfering polymers (e.g. PEO) to disturb the rigid association of
chitosan molecules caused by hydrogen bonding. Co-spinning of bio-polymers
and water-soluble polymers requires the use of cross-linkers for fibre stabili-
sation [25].

7.4 New Developments in Electrospinning

Actual R&D work on electrospinning is focusing on precise control over fibre
size and morphology by changing the process parameters, modelling of the
electrospinning process, the development of new structures and functionalities
of nano-fibres and the development of practical applications of electrospun
fibres.
The working group of Greiner and Wendorff developed a co-electrospinning
procedure enabling the production of core–shell nano-fibres with specialty
properties [13, 14, 20, 58].
Other specialty nano-fibres produced by electrospinning are nanotubes or
fibres with very porous surface structure [14].
Another possibility is the incorporation of nano-particles/micro-spheres
into nano-fibres to achieve special functionality (Fig. 7.12) [14, 59].
136 K. Schaefer et al.

Fig. 7.12. Nano-fibre with incorporated micro-spheres [59]

Big interest in electrospinning of nano-fibres exists in the area of bio-

medical applications [33–36]. Yet 1980, ICI patented a “product comprising
electrostatically spun fibres” produced from polyurethane melts which were
intended to be used as vascular prosthesis [60]. Recently, portable electrospin-
ning equipment was developed which can be applied for wound healing [61].

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