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Towards a new positioncontrolled electrospinning setup

T.A. Baede
DCT 2009.052

Masters thesis
Coach(es):

dr. ir. M.J.G. van de Molengraft


dr. ir. G.W.M. Peters

Supervisor:

prof. dr. ir. M. Steinbuch

Eindhoven University of Technology


Department of Mechanical Engineering
Dynamics and Control Technology Group
Eindhoven, June, 2009

Table of contents
Summary......................................................................................................................................................... 1
Introduction ..................................................................................................................................................... 3
Chapter 1: Electrostatics ................................................................................................................................. 8
1.1: Electric field without dielectric ............................................................................................................. 8
1.2: Refinements ...................................................................................................................................... 10
Chapter 2: Process parameters, materials and cabin ................................................................................... 13
2.1: Process parameters .......................................................................................................................... 13
2.2: Materials............................................................................................................................................ 14
2.3: Electrospinning cabin ........................................................................................................................ 14
Chapter 3: Pre-design experiments .............................................................................................................. 16
3.1: Introduction ....................................................................................................................................... 16
3.2: Experiments and results.................................................................................................................... 16
3.2.1: Fiber deposition: experiments.................................................................................................... 16
3.2.2: Fiber deposition: results ............................................................................................................ 17
3.2.3: Writing: experiments.................................................................................................................. 19
3.2.4: Writing: results........................................................................................................................... 20
3.2.5: Influence of collector thickness: experiments ............................................................................ 22
3.2.6: Influence of collector thickness: results ..................................................................................... 22
3.2.7: Influence of collector-electrode airgap: experiments ................................................................. 24
3.2.8: Influence of collector-electrode airgap: results .......................................................................... 24
3.3: Design implications ........................................................................................................................... 25
Chapter 4: Design of a new electrospinning setup........................................................................................ 26
4.1: Introduction ....................................................................................................................................... 26
4.2: Design requirements ......................................................................................................................... 26
4.3: Configurations ................................................................................................................................... 27
4.4: The cylinder spinner .......................................................................................................................... 29
4.5: Material selection .............................................................................................................................. 30
4.6: Rotation axis ..................................................................................................................................... 30
4.7: Translation axis ................................................................................................................................. 30
4.8: Realisation ........................................................................................................................................ 30
4.9: End stops, homing strategy, endpoint detection................................................................................ 34
4.9: Control design ................................................................................................................................... 35
4.9.1: System identification.................................................................................................................. 35
4.9.2: Inter-axis disturbances .............................................................................................................. 36
4.9.3: GUI and real-time control .......................................................................................................... 36
4.9.4: Feedback control ....................................................................................................................... 37
4.10: Spacing error................................................................................................................................... 40
Chapter 5: Post-design experiments............................................................................................................. 42
5.1: Stationary deposition experiments on glass cylinder......................................................................... 42
5.1.1: Experiments............................................................................................................................... 42
5.1.2: Results ...................................................................................................................................... 42
5.2: Testing with motion ........................................................................................................................... 42
5.3: Troubleshooting ................................................................................................................................ 43
5.4: Stationary deposition experiments on PET ....................................................................................... 46
5.4.1: Experiments............................................................................................................................... 46
5.4.2: Results ...................................................................................................................................... 46
Conclusion and recommendations................................................................................................................ 48
References.................................................................................................................................................... 49

Summary
Electrospinning is a powerful and versatile technique for the fabrication of very thin fibers from
polymer solutions. In contrast to mechanical drawing processes, spinning with an electric field
provides the ability to produce fibers with much thinner diameters, typically in the micro- and
nanometer range.
In a conventional electrospinning process, a polymer solution is fed to a metallic nozzle so that a
drop appears at the tip of this nozzle. A high voltage is then applied to the nozzle, while at some
distance below it a grounded plate electrode is placed. The potential difference between both
points generates an electric field. The drop becomes charged and a thin jet is ejected from the
nozzle. Due to electrostatic forces, the jet is pulled towards the electrode. By placing a thin sheet
of collecting material between nozzle and electrode, the fiber is deposited on this so-called
collector.
Due to instabilities in the process, the material is deposited randomly, forming a so-called
nonwoven mesh with a chaotic structure. For future electrospinning applications in the fields of
filtration, tissue engineering and nano-electronics, it is necessary to make the fiber deposition
controllable. A technique developed at Eindhoven University of Technology consisting of a
moving collector and a thin, positionable grounded needle electrode makes this possible and was
implemented in an electrospinning setup. However to improve fiber deposition control, more
knowledge of the electrospinning process is required. The goal of this research study is to acquire
this knowledge through experiments.
In a first experiment, the deposition mechanisms for the grounded plate and needle electrodes
were studied. It was learned that although the deposition mechanisms are different, the
deposition looks similar. Secondly, PEO and PCL fibers were written on a moving collector
consisting of a mylar sheet in a straight line. Interestingly, it was discovered that both fibers had a
rectangular cross section. In a third experiment, it was investigated whether the collector
thickness influences the amount of deposition. It was discovered that the collector thickness does
indeed play a role and that reducing this thickness leads to more pronounced deposition. This
experimental result corresponds with electrostatic analysis, which suggests that although a
dielectric collector does not change the overall shape of the electric field, it does locally reduce
the field strength. This leads to a decrease in electrostatic pulling force and thus the amount of
deposition. In a fourth experiment, the goal was to find out whether a small airgap between
electrode and collector prevents, hinders or otherwise alters the deposition. No apparent visible
difference was detected in deposition between both types of samples. The airgap did not prevent
or hinder deposition.
Although great strides have been made in the control of the fiber deposition point, there is still a
difference between desired and realized deposition points. To further improve fiber deposition
control, it is imperative to find out which process parameters influence the fiber deposition error.
The current electrospinning setup lacks the required position accuracy to successfully investigate
this. Therefore, a new setup must be designed.
Design requirements for such a new electrospinning setup have been set. Two designs that meet
these requirements were generated, one with a planar and another with a cylindrical configuration.
A cylindrical configuration was determined to be superior and was further developed. It consists
of a rotating, thin-walled glass, cylindrical collector that can also translate along its center axis.
This cylinder spinner was built and equipped with a homing mechanism to enable reproducible
results. Furthermore, a motion control scheme was implemented.

During testing of the new design two problems were encountered:


1. Focusing did not occur on the glass cylindrical collector.
2. The desired collector speed could not be reached due to mechanical problems in the
rotation axis.
Both problems were analyzed. It was discovered that the electrostatic properties of the design are
sound, but that the relatively large wall thickness of the glass cylinder prevented focusing.
Changing the spinning parameters had no effect on focusing. A new glass cylinder with a reduced
wall thickness is unpractical due to issues with ease-of-handling, safety and durability. Through
experiments it was determined that a thin-walled PET cylinder offers significantly better focusing
without any of the before-mentioned complications and could therefore be a viable alternative to
the installed glass cylinder. To address the collector speed problem, it is recommended to use a
polymer that requires a lower collecting speed. Alternatively, the rotation axis could be
redesigned.

Introduction
Electrospinning is a powerful and versatile technique for the fabrication of very thin fibers from
polymer solutions or melts. The resulting fibers are continuous and have a uniform diameter. This
diameter can vary from tens of micrometers down to a few nanometers, depending on the
process parameters. Furthermore, fibers with both solid and hollow interiors can be achieved. It is
also possible to give the fibers special properties by adding metallic, ceramic or even biological
compounds such as proteins or DNA to the source polymer material.
In literature, the technique is often compared to the traditional fiber spinning process where a
polymer melt or solution is extruded through a die with a small hole. In electrospinning, however,
instead of using mechanical forces to form the fibers, electrostatic forces are employed. The
advantage of this contactless drawing is that fibers with significantly smaller diameters can be
produced.
As mentioned before, both polymer solutions and melts can be used as a source material, but in
this report we will focus on electrospinning using polymer solutions.
In a typical procedure (see Fig. 1), a syringe with polymer solution is placed in an infusion pump
to generate a constant flow of fluid through the needle. This needle is connected to a metallic
capillary, the so-called nozzle, with a transport tube. The polymer solution is pumped through the
tube and a small liquid drop appears at the tip of the nozzle. A high voltage is then applied to the
nozzle, usually between 5 and 50 kV, while at some distance below the nozzle a grounded
electrode is placed. The potential difference generates an electric field between nozzle and
electrode.

Charged nozzle
Taylor cone
Jet
High voltage
supply
Syringe
Collecting material

Infusion pump
Grounded electrode

Figure 1: A characteristic electrospinning setup


Due to the electric field, the shape of the drop starts to deform from the shape caused by surface
tension alone to a conical shape called a Taylor cone [1]. When the electric field is sufficiently
high and charge buildup in the cone reaches a critical level, the electrostatic forces will overcome
the surface tension of the polymer solution and a thin, viscoelastic jet is ejected from the capillary
nozzle. Under the action of the electric field, the fibers are forced to travel towards the grounded
electrode. While the charged jet is travelling downwards, the polymer is continuously stretched by
the electrostatic forces. At the same time, the solvent evaporates. The combination of these two
effects results in a significant reduction of the jets diameter.

The jet does not follow a straight path to the electrode, however. Instead, shortly after exiting the
nozzle, a chaotic oscillation occurs, caused by charge repulsion between material elements of the
jet and an aerodynamically driven bending instability. The oscillation is known as the whipping
phenomenon in literature [2]. Because of this phenomenon, the material is randomly deposited,
creating a so-called nonwoven mesh (see Fig. 2). It is also possible to place a thin sheet of
collecting material (also called collector) on the electrode so that the electrospun material is
deposited on this sheet instead of directly on the electrode.

Figure 2: An electrospun nonwoven mesh [32]


Since the structure of the nonwoven mesh is essentially chaotic, its properties are hard to predict
and characterize. Although a random structure is sufficient for some electrospinning applications,
for others one would prefer or even require a better control over how the micro- or nanofibers are
oriented.
Examples of application fields where orientation control could play a key role are: filtration [3, 4],
sensors [5-8], electronics [9, 10] and tissue engineering [11-13]. In the filtration field, the pore-size
of a filter is of prime importance as it determines the flow resistance and selectivity [14]. Making
the fiber spacing in the mesh constant and reproducible would be very desirable. Such control
would also allow researchers in the biomedical field to carefully optimize scaffold structures for
tissue engineering. Finally, when one wants to create highly efficient sensors and electronics
based on nanofibers, well-aligned and highly ordered architectures are required.
Control of the orientation of nanofibers is therefore very desirable and numerous methods with
various levels of success are described in literature. Worldwide, many research groups have
experimented with methods to control the orientation of fibers during electrospinning with various
levels of success. An overview of these methods can be found in Table 1.
The methods can be divided into three groups based on how the orientation is achieved:
mechanically, through electrostatic means or both. We define mechanical as using movement (i.e.
rotation and/or translation) inside the setup to accomplish alignment, focusing and positioning of
the fibers. When this is achieved solely through the shape of the setup, we define this as
electrostatic. Finally, if both means are important for the end result, we classify the method as
such.
The results from literature will be compared on two qualitative fronts: alignment and controllable
spacing.

Aluminium foil on rotating cilinder

Liquid bath-as-collector

X
X
V
V
V
X
V

Electrostatic lens as focusing element

Cylindrical auxiliary electrode

Auxiliary electric field

Electrode-gap spinning

Metal frame electrode

Knife-edge electrode in needleless spinning

Metal grid collector

V
V

Knife-edged blade electrodes

Aluminium foil on rotating cilinder /w copper electrodes

Scanning tip spinning


V

X,Y,Z-positioned collector

Cylinderspinner

Parallel grid of aluminium strips as electrode

Bobbin collector

Near-field electrospinning

Copper wire drum collector

Both:

Ring auxiliary electrode

Electrostatic:

V
X

Rotating disk collector

Alignment

Rotating wooden or aluminum frame as collector

Mechanical:

Method

Table 1: Orientation control methods in literature

Controllable spacing

Bhattarai

Teo

Teo

Sun

Kameoka

Mitchell

Sundaray

Theron/Zussman

Katta

Gibson

Yarin

Dersch

Li/Xia

Huang

Kim

Deitzel

Jaeger

Smit

Bhattarai

Subramanian

Huang

Author

[31]

[30]

[30]

[29]

[28]

[27]

[26]

[25]

[24]

[23]

[22]

[21]

[20]

[15]

[19]

[18]

[17]

[16]

[13]

[12]

[15]

Ref.

Alignment is defined as whether there is control over how parallel all fibers are positioned to each
other.
Controllable spacing is defined as whether or not it is possible to deposit two fibers next to each
other with a controllable spacing between them.
From the results in Table 1, it follows that achieving alignment of nanofibers along a single axis is
currently well-understood. The controllable spacing, however, is a different issue. Only two
groups, [27] and [29], report that they can carefully control the distance between two fibers.
At Eindhoven University of Technology, a new technique has been devised and patented to
carefully control the position of the fiber deposition point. Instead of using a grounded plate as
electrode, a grounded needle is used which can be actuated in the plane (see Fig. 3). This
technique can potentially improve the alignment and degree of spacing control significantly.
The feasibility of the technique was demonstrated by Solberg [32]. He also implemented the
technique in an experimental setup and showed that it is possible to align and deposit a single,
continuous fiber on the collecting material by moving the collector with respect to the electrode.
Fig. 4 shows a glass sample with neatly aligned electrospun fibers deposited on it using this
setup.
The experimental setup by Solberg has provided much insight into the electrospinning process.
Due to its components, however, the attainable position accuracy of the electrode and collecting
material is limited and this prevents the precise fiber deposition that is required for advanced
oriented fiber meshes necessary for many future applications. Therefore, a new electrospinning
setup is required.

Figure 3: Overview of new electrospinning technique


using an actuated grounded needle electrode
In this project, the following goals have been set:

Acquire more knowledge of the fiber deposition process for future improvements of
orientation control.

Design, build and test a new electrospinning setup with higher position accuracy than the
current one which is capable of depositing straight fibers with an adjustable spacing in a
reproducible manner.

Figure 4: Electrospun fiber spirals on a glass disc with a spacing of 1 mm [32]


This work will start with a description in Chapter 1 of the electrostatic mechanisms that play a role
in electrospinning. Then, a short overview is given of important process parameters, studied
polymers and equipment in Chapter 2.
A number of experiments were performed to obtain more knowledge of the fiber deposition
process. These will be discussed along with results in Chapter 3. The design of the new
electrospinning setup and its real-time motion control is addressed in Chapter 4. In Chapter 5,
tests performed with the new setup are described. Finally, conclusions are drawn and
recommendations for future work given.

Chapter 1: Electrostatics
In order to control the location of material deposition and improve deposition accuracy, good
knowledge of the underlying electrospinning process is required. Key to this control is the electric
field. First, the overall shape of the field is discussed based on electrostatics. Thereafter, a
number of effects that also influence the shape will be described to refine the situation description.
1.1: Electric field without dielectric

From an electrical standpoint, the electrospinning setup is composed of two elements: the
charged nozzle at the top and the grounded needle electrode at the bottom. This situation can be
modeled as an electric dipole. It consists of two point sources of charge, one at the tip of each
element, with a certain separation distance h. A positive charge is applied to the nozzle; hence
negative charge accumulates on the electrode to maintain equilibrium. The potential difference V
between both elements is kept constant.

Figure 5: (a) Electric field for two point sources. Blue lines represent the field lines with
the arrows indicating the direction of the electrostatic force. Red contour lines represent
the equipotential lines. (b) The same plot, but incorporating a dielectric collector.
In Fig. 5a, the shape of the electric field is shown. The red dashed contour lines represent the
equipotential lines. As the name suggests, all points on such a line are at the same electric
potential. The nozzle is at the maximum potential, while the electrode is at zero potential due to
grounding. Hence, the potential decreases while moving downwards from one equipotential line
to the next. The blue solid lines represent the electric field lines and are always perpendicular to
the equipotential lines. By convention, the direction of the lines is from positive to negative charge.

The closer the field lines are to each other, the stronger the field in that region. The field is thus
strongest near nozzle and electrode.
The relationship between potential difference and electric field strength is given by:

r r
V = E dl
b

(1.1)

Here V is the potential difference between the nozzle at location a and the electrode at location b

in [V]. E is the electric field strength in [V/m] and dl is an infinitesimal increment of


displacement on any line or curve between both points [m].
When we assume the electric field is uniform over the separation distance, like between two
charged parallel plates where fringing is ignored, the magnitude of the electric field strength can
be estimated using:

E=

V
h

(1.2)

with h in [m].
From this equation it can be concluded that the electric field strength is highest on the vertical
field line since the field line is shortest. In order to investigate what this means for the
electrospinning process, assume that a positive test charge is inserted in the field. The force that
this test charge will experience can be calculated from:

r
r
F = QE

(1.3)

with the force F in [N], the test charge Q in [C] and the strength of the electric field E in [V/m].
The electrostatic force acts in the direction of the electric field and therefore the pulling force on
the vertical field line will be highest. All field lines converge towards the electrode and thus the
point of the needle there will exert the largest pulling force.
Although in reality the electric field is clearly not uniform over the distance, the order of the field
strength can be estimated with Eq. 1.2. When we enter a characteristic V = 12 kV and
5
h = 0.1 m, we arrive at a field strength of E = 1.210 V/m. This is one order of magnitude below
6
the dielectric strength of air, Ebreakdown = 3.0 10 V/m, which is the field strength at which air
becomes electrically conductive [33]. The breakdown phenomenon puts a limit on how far the
field strength can be increased to accomplish focusing.
In the above text, we started from point charges. However, in reality both electrical elements have
finite dimensions and their shape influences how the electric field looks like. In Fig. 6, the electric
field around real needle or nozzle configurations is shown. The equipotential lines wrap around
the contour of the nozzles.

Figure 6: Electric field around two nozzle configurations:


(a) An isolated nozzle. (b) A nozzle attached to a horizontal plate.

1.2: Refinements
Field with dielectric:
In the electrospinning setup, we use a dielectric, which we have called collector to capture the
spun polymer fibers. When a dielectric is inserted in an external electric field, the shape of the
overall electric field is not influenced, see Fig. 5b. Only within the dielectric itself, the electric field
will change. This effect is called polarization. The externally applied electric field will induce some
separation of charge in the dielectric molecules. Negative charge will orient itself towards the
upper boundary of the dielectric; positive charge orients itself towards the lower boundary of the
dielectric. Therefore, the net effect is as if there is a negative charge on the upper surface and a
positive charge on the lower surface of the dielectric. A close-up of the dielectric, demonstrating
the polarization effect, can be seen in the following figure:

Figure 7: Molecular view of polarization within a dielectric

The field in the dielectric E d is a vector sum of the externally applied field E ext and the field

r
Eind due to the induced charge on the surfaces of the dielectric:
r
r
r
E d = E ext + Eind

(1.4)

The strength of the induced field is given by a function:

r
r
Eind = f ( 0 , P)
The exact definition depends on the geometry of the dielectric. In this equation,

r
2
2
2
constant of vacuum [C /Nm ] and P is the polarization density vector in [C/m ].

(1.5)

0 is the dielectric

The level of polarization that occurs can be calculated from the following relation:

r
r
P = 0 e Ed

(1.6)

where e is the electric susceptibility of the dielectric [-]. Note that the polarization depends on the
total electric field inside the dielectric.
Since in the electrospinning setup the induced field and external field are in opposite directions,
the field in the dielectric Ed is weaker than the external field Eext.

10

In the discussion above, we assumed that the dielectric is one layer of a single material. When
the collector consists of two or more layers of different materials, then

r
Eind in those layers will

differ from each other. However, as for one layer, the shape of the electric field outside of the
dielectric will not be influenced.
The same holds for a collector that is not positioned exactly halfway between nozzle and
electrode, but closer to one of the two. Although the field within the collector is no longer uniform,
the electric field outside the dielectric will keep its shape.
Introduction of the polymer:
During the electrospinning process, a drop of polymer solution is elongated and guided towards
the grounded electrode by a combination of gravity and electrostatic force. Since the polymer
solution is charged, in essence it can be seen as an extension of the nozzle. When the material
moves towards the dielectric, this is equivalent to the dielectric moving towards the nozzle.
The distance between the upper needle and dielectric decreases and thus the electric field
strength and consequently the electrostatic force increases. This leads to a distortion of the
electric field (see Fig. 8a). However, since the accumulated charge is hard to measure, the
amount of field distortion is currently unknown.
Nozzle with polymer
Nozzle with polymer

Dielectric

Dielectric

(a)
(b)
Figure 8: (a) Distortion of the electric field due to presence of polymer. (b) Contact
situation.

While the material travels downwards in the form of a jet, the solvent evaporates. Consequently,
the conductive properties of the jet change, as the material changes from a solution to a solidified
polymer.
Contact situation:
When the polymer fiber comes into contact with the dielectric, a new situation occurs. A current
will start flowing through the conductive polymer fiber.

I = Qv + E

(1.7)

where Q is the charge [C], v is the polymer flow velocity [m/s], the conductivity [m/] and E the
electric field strength [V/m].
The first term represents transport of charge due to movement of the polymer. The second term
is conduction following Ohms Law. Whether this latter term plays a role depends on the
conductive properties of the polymer when it comes into contact with the dielectric.

11

Since the collector is fabricated from an electric isolator, the charge deposited by the polymer
cannot flow away (see Fig. 8b). Therefore, the collector will become locally charged because of
the presence of charged fiber segments. These deposited segments will repel newly spun
material that arrives at the collector. On a flat collector, this leads to a radially expanding drop of
solidified polymer as this distributes charge in the most optimal way [32]. The repulsion effect is
expected to be localized; however experiments are necessary to confirm this hypothesis.
The dielectric will not stay charged forever, however, as charge will diffuse into the surrounding
atmosphere. Therefore, deposited segments will gradually lose their charge.

12

Chapter 2: Process parameters, materials and cabin


Position-controlled electrospinning is a complex process and requires knowledge of
electrohydrodynamics, chemistry, rheology and motion control to operate and fully address its
potential.
2.1: Process parameters
Many parameters play a role in the electrospinning process. These can be broken down in
material properties and operational parameters:
Material properties of the polymer:

Molecular weight
Molecular weight distribution
Architecture, such as linear, branched, etc.

Material properties of the solution:

Viscosity
Electrical conductivity
Surface tension

Operational parameters:

Electric field strength E


Polymer solution feed rate f
Distance between nozzle and collector d
Distance between collector and electrode (airgap) a
Velocities of the nozzle, collector and electrode
Ambient parameters (temperature, humidity, cabin air velocity)

The electric field strength is determined by the applied voltage V and the layout of the setup.
The deposition time period t plays a role in the characteristics of the produced mesh. A number
of operational parameters are shown in Fig. 9.

Figure 9: Operational parameters

13

2.2: Materials
As mentioned in the first Chapter, the research described in this report focuses on using polymer
solutions for electrospinning. A solution is made by dissolving polymer powder in a suitable
solvent. Huang [3] lists over forty different polymers that have been electrospun in solution form
using a wide range of solvents. In this research project, two polymer solutions were used
extensively. These are listed in Table 2.
Table 2: Used polymer solutions
Polymer
Molecular weight
PEO (Polyethylene oxide)

400,000

PCL (Polycaprolactone)

200,000

Solvent
Distilled water / ethanol
(2:3)
Chloroform

Concentration
8 wt%
18 wt%

Polyethylene oxide solution is by far the most used material in electrospinning studies as it is
relatively simple to prepare and use. Therefore, a lot is known about this material, its behaviour
and properties. For these reasons, PEO was selected as main component of this research.
Polycaprolactone is a biodegradable polymer used extensively in tissue engineering research,
which is one of the proposed fields of application for oriented fiber meshes. A drawback of this
material is that it is commonly dissolved in chloroform, which evaporates during electrospinning
and leads to harmful gas formation. As a result, the use of PCL solution was limited in this project.
2.3: Electrospinning cabin
All experiments have been performed in a dedicated cabin (see Fig. 10). This cabin is outfitted
with a high voltage supply that can be controlled from an operating panel. It also protects the user
from a number of risks.

Figure 10: Electrospinning cabin [32]

14

One risk is the high voltage (up to 25 kV). When a user accidently comes into contact with an
electrified element of the setup, the voltage enables a current to flow through the body which is
harmful and could potentially lead to death. Therefore, the cabin, which is equipped with a door
that provides access to the electrodes and other parts of the setup placed inside, is outfitted with
a safety mechanism that shuts down the voltage when the door is opened.
In the previous Paragraph it was mentioned that harmful gases may be produced during
electrospinning. Therefore, the cabin is connected to a forced ventilation system that captures
and leads any emitted gases away from the setup.

15

Chapter 3: Pre-design experiments


In this Chapter, an overview will be presented of all experiments that were performed to obtain
more knowledge of the electrospinning process and to assist in the design of a new
electrospinning setup. Additionally, the results of these experiments will be analyzed and
discussed.
3.1: Introduction
In the work of Solberg [32], the feasibility of focusing the fiber deposition by using a thin grounded
needle electrode instead of a grounded plate electrode was shown through experiments.
Furthermore, it was demonstrated that a single straight fiber could be produced by applying a
velocity difference between collector, nozzle and electrode. These experiments will be taken as
starting point of this investigation to gain more insight into the electrospinning process.
3.2: Experiments and results
In the following sections, four sets of experiments will be performed. The goal of the first set of
experiments, described in Paragraph 3.2.1, is to compare the mechanism of fiber deposition on a
grounded plate electrode with that on a grounded needle electrode. In Paragraph 3.2.3, the
deposition on a moving collector is investigated. The goal of this experiment is to determine
whether fibers can be written with both PEO and PCL and if so what the properties are of these
fibers. Then, in Paragraph 3.2.5, a set of experiments is described to determine whether the
collector thickness influences the amount of deposition. The goal of the last set of experiments,
described in Paragraph 3.2.7, is to find out whether a small airgap between collector and
electrode prevents, hinders or otherwise alters the deposition.
3.2.1: Fiber deposition: experiments
As mentioned previously, the goal of the first set of experiments is to compare the mechanism of
fiber deposition on a grounded plate electrode with that on a grounded needle electrode.
In the first test, a thin, blunt 23G Terumo injection needle with an inner diameter of 0.337 mm is
positioned in a brass holder. The combined needle and holder will be called nozzle henceforth.
This nozzle is placed in a stand with a variable height and connected to the plus terminal of the
electrospinning cabins high voltage supply. Directly below the nozzle, a circular, copper plate
electrode with diameter of 5 cm is placed. The plate electrode is connected to the minus terminal
of the cabin. A Harvard PHD 2000 infusion pump is used to feed PEO solution (see previous
Chapter for properties) to the nozzle via a Teflon tube. Thin mylar sheets (thickness of 0.01 mm)
and thin glass samples (thickness of 0.55 mm) are used as collecting material and placed in
direct contact with the grounded plate electrode. In Fig. 11a, the setup used for this test is
depicted.
As preparation for the experiment, the infusion pump is switched on so that a constant feed of
polymer solution begins to flow through the tubing. During experimentation, the pump is never
turned off as the polymers under study are viscous and we want to minimize transient behaviour
of the fluid. Once the solution is ejected in a steady-state manner from the nozzle, experiments
can take place. Paper covering that keeps the electrode clean is removed and the collecting
material is placed on the electrode. The experiment starts when an uniform drop has formed and
the high voltage is applied. After spinning for a set duration, the high voltage is switched off, the
collecting material removed and the cabin and equipment cleaned with ethanol to remove any
remaining charged polymer strands that could disturb subsequent experiments. All experiments
are performed at ambient cabin temperature (22.4C) unless noted otherwise.

16

Figure 11: Fiber deposition setup. (a) With grounded plate electrode. (b) With grounded
needle electrode.
In the second test, the plate electrode is exchanged for a grounded, conical-shaped needle
electrode with an outer diameter of 0.9 mm (see Fig. 11b). All other elements of the setup and
procedure are kept the same.
For these tests, the spinning parameters are chosen such that a stable polymer jet is established
and deposition is clearly visible. Note that the main focus of the present tests is not to compare
deposition for different parameters, but rather to assess the deposition mechanisms that occur.
In the following table, the spinning parameters for both tests are summarized for reference, where
V is the applied voltage in kV, f is the polymer solution feed rate in [l/min], t is the time period in
which deposition occurs in [s] and d is the vertical distance between nozzle tip and collecting
material in [cm].
Table 3: Spinning parameters for fiber deposition experiments
Experiment
Electrode type
Collecting material
V [kV] f [l/min]

t [s]

d [cm]

1
2
3
4

120
120
60
120

13
13
12
12

plate
plate
needle
needle

mylar
glass
mylar
glass

17
17
17
17

18
18
18
8

These tests are different from those described by Solberg [32] as a higher V and different values
for f have been used. Furthermore, in this research both mylar and glass are studied, while [32]
solely studied mylar.
3.2.2: Fiber deposition: results
The first results that will be discussed are those of the fiber deposition experiments.
In experiments 1 and 2, where a plate electrode is used, it is observed that the polymer jet is
ejected straight down from the Taylor cone. Several centimeters above the collecting material, the
jet starts to diverge from its vertical path and an oscillating haze is observed. The first segment of
the incoming polymer has no preference for a specific point of the plate electrode and is thus
deposited randomly on the collecting material. Upon deposition, the segment retains a residual
charge that exerts a repulsive force on subsequent segments and sweeps them to another
location. As a result, the collecting material is covered with randomly deposited fibers that

17

ultimately form a nonwoven fabric. Images of these results are shown in Figs. 12.1 and 12.2,
respectively. Note that special care was taken to visualize the delicate fiber deposition using
optimal camera angles and with optimal lighting conditions and these might differ from sample to
sample. The mylar sheets and glass samples shown in the images of this Chapter are
occasionally kept up with black foam tubing or a combination of thin white and red strips and pins
to facilitate photography. These aids are not important and should be ignored. The bright, little
drops in the center of the photographs in this Chapter are caused by the initial polymer drop when
the voltage is applied or the last drop after the voltage has been removed. They are not part of
the main deposition process we want to study and should therefore be ignored.

Figure 12: Photographs of collecting materials after deposition experiments


Different behaviour is observed in experiments 3 and 4 where a needle electrode is used (see
Figs. 12.3 and 12.4, respectively). The whipping phenomenon is significantly reduced and,
although some haze is observed, the fiber is first collected very close to or, under ideal conditions,
exactly above the needle electrode. The circular deposition spot grows in diameter with time. This
can be explained by the fact that the fiber, which has been deposited on the sheet, retains an
amount of residual charge which exerts a repellant force. After the first fiber segment has been
collected, the continuous deposition leads to pile up of new fiber material at the initial deposition

18

point which ultimately buckles. The already deposited fiber segments charge pushes the new
fiber away to another location. As more fiber is collected, the repellant forces will direct new
material further out of the center of the deposition spot. The spot remains circular, however, since
the needle electrode is still attracting charged fiber segments. From these experiments, it can be
concluded that a needle electrode focuses fiber deposition. After a limited time, material is no
longer deposited directly above the electrode because of repulsive forces. A solution to this
problem is to move already deposited fiber segments away from the deposition point and put
untouched collecting material in the path, so that incoming fiber segments stay attracted to the tip
of the needle electrode and focusing is maintained.
All photographs show similar circular deposition although the deposition mechanisms of a plate
electrode and a needle electrode, as described earlier, are clearly different.
3.2.3: Writing: experiments
In the previous section, focusing on a stationary collecting material was investigated. To obtain a
single straight fiber and create oriented fiber meshes, however, it is necessary to create a velocity
difference between nozzle and electrode on one hand and the collector on the other hand. In this
simple test, the grounded needle electrode setup introduced earlier is reused. PEO and PCL will
be selected as polymer solutions. The same experimental procedure is followed with the
exception that a long strip of mylar sheet is used which protrudes from the electrospinning cabin
through a slit on one end. During electrospinning, the strip is manually pulled further out of the
cabin with a velocity of several cm/s. In this way, the mylar translates over the needle electrode
while it keeps in direct contact with it (see Fig. 13). Deposited fiber is thus transported away from
the deposition point above the electrode and we expect that focusing is maintained.

Figure 13: Writing experiment


The writing experiment is prepared by varying the spinning parameters and selecting those that
yield the most pronounced polymer tracks on mylar for both polymers. After selection, the
writing test is performed three times for PEO and one time for PCL with the following parameters:
Table 4: Spinning parameters for writing experiments
V [kV]
f [l/min]
Polymer solution

d [cm]

PEO
PCL

13
7

20
22

18
30

19

3.2.4: Writing: results


In Fig. 14, a photograph of the mylar sheet used in the PEO writing test is shown. In this image,
two nearly vertical white lines can be seen, marked with two white arrows. These lines are the
parallel polymer tracks written on the sheet. The left track is curved over the bottom half of its
length because it was not pulled in a entirely straight, continuous motion. The right track however
is significantly better due to better steering of the sheet. It is observed that the polymer fiber is
deposited in an entwined, thread-like fashion as the horizontal velocity of the sheet is too low to
collect the fiber as a straight, single fiber.
The result of the PCL writing test is presented in Fig. 15. Here, only one polymer track was spun,
again marked with white arrows.

Figure 14: Writing test result for PEO. Height of image = 10 cm.

Figure 15: Writing test result for PCL. Length of image = 12 cm.

20

From these experiments, it is learned that it is possible to write polymer tracks on mylar sheets.
These results correspond with those of Solberg [32]. By increasing the collection velocity, it
should therefore be possible to write a single, straight fiber on a collector.

Figure 16: Topography of PEO sample

Figure 17: Topography of PCL sample


To learn more about the properties of these fibers, the samples were analyzed with confocal
microscopy and interferometry using a Sensorfar PLu 2300 optical imaging profiler. Several
locations along the fiber were selected and the diameter was measured. Interestingly, the
measurements showed that the fibers did not have circular cross sections, but rather a

21

rectangular shape. The PEO fibers had a height of 380 nm and a width of 8 m, thus a h:w ratio
of 1: 21. The PCL fibers had a height of 14 m and a width of 27 m, which is a h:w ratio of
approximately 1:2. Results are shown in Figs. 16 and 17 for PEO and PCL, respectively.
3.2.5: Influence of collector thickness: experiments
One research question that has not been properly addressed in electrospinning research at
Eindhoven University of Technology is whether the collector thickness influences the amount of
deposition. To investigate this question, the grounded plate electrode setup will be used and
strips of glass and polycarbonate with varying thickness are used as collector material and placed
directly on the electrode, while all other spinning parameters are kept constant. The amount of
deposition on the samples will then be compared qualitatively. The plate electrode is chosen over
the needle electrode as the former gives a more pronounced deposition effect in the same time
frame.
Different collector thicknesses lead to different nozzle-collector distances when the vertical
distance between these two points is not adjusted. It is assumed for these experiments that this
difference of a few millimeters is negligible when considering a vertical distance of 5-15 cm and
will not lead to different electrospinning behaviour.
Four experiments will be performed, as two polymer solutions (PEO and PCL) and two collector
materials (glass and polycarbonate) will be investigated. For each experiment, either two or three
collector thicknesses are compared. In the following table, the spinning parameters are
summarized. Here t1, t2 and t3 are the thickness of the collectors that are compared in [mm].
Table 5: Spinning parameters for collector thickness experiments
V [kV]
f [l/min]
d [cm]
t1 [mm]
t2 [mm]
t3 [mm]
Experiment
17
Experiment
17
Experiment
12
Experiment
12

1: PEO with glass as collector material:


18
13
0.55
1.1
2: PEO with polycarbonate as collector material:
18
13
1.0
3.0
3: PCL with glass as collector material:
17
7.8
0.2
1.4
4: PCL with polycarbonate as collector material:
17
8.4
1.0
2.0

t [s]

120

120

60

3.0

60

3.2.6: Influence of collector thickness: results


In Fig. 18, an image of the first experiment is shown. The glass sample on the left has a collector
thickness of 0.55 mm, while the sample on the right has a collector thickness of 1.1 mm. In the
photograph, it can be observed that the PEO deposition on the left sample is denser and optically
whiter than on the right sample.
The results of the second experiment are shown in Fig. 19. The deposition is marked with black
circles. This experiment was performed using polycarbonate as collector and it was observed that
it is a lot harder to spin on polycarbonate than glass as it seems to repulse incoming polymer jets.
When we compare deposition on both samples, the thinnest strip of polycarbonate (shown on the
left) is covered with the most polymer deposition.
The results for PCL are more pronounced than those for PEO. In Fig. 20, two circular glass
samples are shown with a thickness of 0.2 mm on the left and 1.4 mm on the right. The density of
polymer on the left sample is significantly higher and the deposition is more focused than on the
right sample where it appears more spread out, even though the plate electrode is used for both.

22

Figure 18: Collector thickness - experiment 1


Left: t = 0.55 mm. Right: t = 1.1 mm.

Figure 19: Collector thickness - experiment 2


Left: t = 1.0 mm. Right: t = 3.0 mm.

Figure 20: Collector thickness - experiment 3


Left: t = 0.2 mm. Right: t = 1.4 mm.

23

Fig. 21 shows the results of the last experiment where polycarbonate is used as collector in three
thicknesses. The deposition is marked with black circles. Again we observe that the thinnest
sample is covered with the most polymer fibers and this amount of deposition diminishes nicely
with increasing collector thickness.
From these experiments, it can be concluded that the collector thickness does indeed play a role
and reducing this thickness leads to a more pronounced deposition. This can be understood by
taking into account that the collector partially shields off the electrode and thus locally reduces the
field strength. It acts as a sort of resistor in the field. This reduces the electrostatic pulling force
and therefore the amount of deposition. The shape of the overall field is not changed, however.

Figure 21: Collector thickness - experiment 4


Left: t = 1.0 mm. Middle: t = 2.0 mm. Right: t = 3.0 mm.
3.2.7: Influence of collector-electrode airgap: experiments
Another interesting question is whether a small airgap between collecting material and electrode
prevents, hinders or otherwise alters the deposition. To address this question, the grounded
needle electrode setup is used. PEO solution is selected as polymer source and mylar as
collecting material. We will compare deposition on samples in direct contact with the electrode to
deposition on samples with a small collector-electrode airgap a of 1 or 2 mm. The applied voltage
V is set to 17 kV, the polymer solution feed rate f to 18 l/min and the deposition period t was
kept constant at 60 s.
Four experiments will be performed. In each experiment, deposition on a sample in direct contact
with the electrode is compared to one with an airgap, while all other conditions are kept the same.
The parameters are summarized in the following table:
Table 6: Spinning parameters for airgap experiments
Experiment
d [cm]

a [mm]

1
2
3
4

1
1
1
2

12
13.5
13.5
13.5

3.2.8: Influence of collector-electrode airgap: results


All four experiments show similar results. However, to conserve space only one representative
result will be presented. Photographs of the first experiment are presented below. In Fig. 22a, the
result for direct contact is shown, with the result for a 1mm airgap in Fig. 22b.

24

Both pictures show a similar circular deposition with some fibers that are deposited radially
outward from the deposition point on these 6 x 6 cm mylar sheets. One possible explanation of
the deposition of this radial arrangement is that the fibers are created when the area immediately
above the needle electrode is covered with deposition. The electrode is essentially shielded off
and thus the polymer jet follows the electrostatic field lines which now curve from nozzle towards
electrode over the edge of the mylar sheet. The fibers dry before reaching their ultimate target.

Figure 22: Characteristic result of airgap experiment


Two conclusions can be drawn from these results:
1. No apparent visible difference was detected between deposition on mylar where there
was direct contact and where an airgap between mylar collector and needle electrode
existed.
2. The airgaps used in this section do not prevent focusing of polymer nor hinder deposition
on the mylar collector.
3.3: Design implications
From the experiments in this Chapter we have learned several things that are important when
designing a new electrospinning setup:

The collector should be as thin as possible to maximize focusing power.


A small airgap between collector and electrode of 1 or 2 mm does not hamper focusing.

25

Chapter 4: Design of a new electrospinning setup


4.1: Introduction
To achieve the precise fiber deposition necessary for advanced oriented meshes, a new
electrospinning setup is required with a significantly higher position accuracy of the deposition
point than currently available. In this Chapter, the design requirements of such a setup are
presented. Subsequently, a number of potential configurations are generated and evaluated.
Then, one design is chosen and elaborated. Finally, motion controllers are designed and a
graphical user interface is constructed that controls the spinner in real-time.
4.2: Design requirements
The new design should meet the following requirements:
1. Collecting speed 8 m/s
The goal of this project is to create an electrospinning setup capable of depositing
straight fibers with adjustable spacing in a reproducible manner. The straightness of
fibers depends on the velocity difference between the nozzle and electrode on one hand
and the collector on the other hand. If this velocity difference is too low, an entwined
thread is produced instead of a single, straight, continuous fiber. For PEO, the polymer
solution we would like to study, Solberg [32] showed that this speed difference must be at
least 8 m/s for the spinning parameters he used. In order to be certain that straight fibers
are producible, the new electrospinner should be able to reach this collecting speed.
2. Nozzle and electrode placed in-line
In the electrospinning process, a charged polymer fiber flows from the nozzle to the
electrode. The fiber needs to be deposited on the collector exactly above the electrode.
When the nozzle and electrode are not in-line (see Fig. 23), a deposition error occurs.

nozzle
desired deposition point
collector
actual deposition point

electrode

Figure 23: Deposition error


This is because, first of all, sideways bending of the fiber is limited and breakup occurs
for excessive misalignment of nozzle and electrode. Secondly, the charged material
follows the electrostatic streamlines which do not flow through the desired deposition
point. To make the deposition process as simple as possible, it is desirable to have the
charged fiber travel directly downwards from the nozzle toward the electrode. To
minimize the deposition error, the nozzle and electrode should therefore be in-line and
mechanically coupled, for instance by a shared support structure.
3. Minimize influence on electric field
As mentioned before, the electric field determines where a nanofiber is deposited. Hence,
to ensure a proper working of the setup, the disruption of the electric field should be
minimized. Therefore, all design components should either be made of electric isolators

26

or, where this is not possible, these conducting elements should be shielded off.
4. Compatible with existing infrastructure
Electrospinning experiments are always conducted in a dedicated cabin which protects
the user from exposure to high voltages and is outfitted with a dedicated ventilation
system. The new electrospinner should fit within this existing cabin. The maximum
dimensions of the new design are therefore: length < 0.48 m, width < 0.66 m, height <
0.56 m.
5. Spinnable area at least 0.12 x 0.12 m
A spinnable area of at least 0.12 x 0.12 m is desired, based on application considerations.
The fibers are to be positioned as parallel lines with an adjustable spacing s in[m].
4.3: Configurations
With the before-mentioned requirements as constraints, a number of designs were generated.
In order to fulfill the first and second requirements simultaneously, there are two practical options:

A stationary collector and a moving pair of nozzle and electrode.


A moving collector and a stationary pair of nozzle and electrode.

The nozzle and electrode need to be mechanically coupled, for instance by a U-shaped frame.
When we select the first option, the frame will have to move. To study the deposition behaviour,
this option would require a moving camera which is not practical. Therefore, the second option is
selected.
Now that the moving and stationary parts are known, a collector configuration can be selected.
Essentially, there are two configurations that fit the requirements mentioned above: planar and
cylindrical (see Figs. 24a and 24b, respectively).

x&

x&

y&

Figure 24: Collector configurations


The planar configuration consists of a flat rectangular collector which is actuated in the x,y-plane
just above a needle electrode. A mylar sheet of the same size is to be placed on the collector to
capture the fiber deposition. Another solution is to use a configuration where a thin-walled, hollow
cylinder with one open end and radius R is used as collector, which can rotate and translate
along its center axis. A needle electrode is mounted on an arm that sticks into the cylinder. Now,
a mylar sheet of the same size as the collector will be wrapped around it. After electrospinning,
the sheet will be unwrapped.

27

A truly two-dimensional mesh with spacing s can only be woven with a planar configuration (see
Fig. 25). Note that the fiber will only be straight if it is deposited at the required collecting speed.
Therefore, in the planar case, there is an effective spinning area where the collecting speed is
reached and an area outside where it is not. A major disadvantage of this configuration is that a
collector speed of 8 m/s in the plane is hard to achieve. Especially within the limited confines of
the electrospinning cabin which places rather extreme requirements on the acceleration of the
collector when we want to be able to spin with a constant speed for at least 120 mm. This can be
seen by calculating the available acceleration length:

l acc =

l l eff

(4.1)

here l is the width of the electrospinning cabin in [m], leff is the length over which spinning should
occur with a constant velocity in [m] and lacc is the length available for acceleration in [m].
Entering the corresponding values in Eq. 4.1 yields: lacc = 0.27 m.

leff

s
Figure 25: Schematic of a mesh produced with a linear configuration
The required acceleration follows from:

&x&req =
with

V2
2l acc

(4.2)

&x&req the required acceleration in [m/s2] and V the collecting speed in [m/s]. This gives

&x&req = 119 m/s2. This required acceleration puts very high demands on the actuators.
If we only want parallel fibers, it is possible to use a fast axis to deposit the fiber along the length
of the collector and a short axis to move this axis sideways over a distance that corresponds to
the spacing. However, one fast actuator is still required.

b = 2R

s
Figure 26: Schematic of a mesh produced with a cylindrical configuration (folded out)
Using a cylindrical configuration, the collector is rotated with a surface velocity of 8 m/s.
Translation of the collector is necessary to achieve the spacing and fibers will appear as spirals

28

on the collector. In Fig. 26, a schematic of a mesh produced with the cylindrical configuration is
shown. Note that in this configuration, the cabin dimensions are no longer a constraint when it
comes to the collecting speed. As can be seen in the figure, the width of the mesh b in [m] is
equal to the circumference of the cylinder and thus depends on the radius R in [m]. The required
angular velocity req in [rad/s] to achieve the collecting speed is also dependant on the radius.
Taking all design requirements into account, we select R = 0.02 m. This results in
req = 400 rad/s = 3820 rpm. The required angular acceleration can be set freely as it depends
on how long the spinner is allowed to spin up to the required angular velocity.
Now that the rotation of the cylinder has been investigated, attention can be focused on the
translation. It can be gathered from Fig. 24b that the interfiber spacing s that is realized depends
on the collecting speed V and the selected translation velocity x& . Suppose that x& = 0 and V > 0 ,
then vertical polymer lines will appear. When V = 0 and x& > 0 , horizontal lines will appear.
When V and x& are chosen equal, a 45 line is deposited (see also Fig. 26). Hence, for an arbitrary
angle , we can write:

tan( ) =

V
x&

(4.3)

From this same figure, it can be concluded that the deposition angle can also be expressed in
the spacing:

tan( ) =

2R
s

(4.4)

Combining Eqs. 4.3 and 4.4 leads to:

s=

2Rx&
V

(4.5)

With Eq. 4.5 it is possible to calculate the spacing s for a certain translation velocity of the
cylinder. This equation can also be rewritten to obtain the translation velocity as a function of
spacing:

x& =

Vs
2R

(4.6)

4.4: The cylinder spinner


After comparing both configurations, the cylinder configuration is selected. Now, the new
electrospinner can be designed in detail. A concept drawing is shown in Fig. 27. The stationary
part consists of a tower from which a nozzle arm and electrode arm protrude. The translating part
consisting of the cylinder and its drivetrain will slide over the electrode with a small airgap of
1 mm between cylinder interior and electrode. Several actuator mechanisms were considered
and a ballscrew drive was selected. The translating part of the spinner will be mounted on this
drive.

29

Figure 27: Cylinder spinner concept drawing (translation mechanism not shown)
4.5: Material selection
The rotating cylinder will be made from glass with a wall thickness of 2.5 mm. The material is an
electric isolator, readily available, easy to machine and resistant to aggressive solvents which are
occasionally used in electrospinning.
The frame of the cylinder spinner is built from thick polymer sheets. Polyvinylchloride (PVC), with
its good electric isolation properties, was selected for the majority of frame. Polyetheretherketone
(PEEK) was chosen for the electrode arm and polycarbonate (PC) for the nozzle arm because of
the shape retention and moisture resistance properties of these materials.
4.6: Rotation axis
At one of the endpoints of the glass cylinder, a PVC plug is inserted and connected to a Maxon
RE25 (type 118746) electromotor. A WM Berg bellow coupling is used to prevent alignment
problems. The electromotor rotates the cylinder up to 3820 rpm, which corresponds with 8 m/s.
The cylinder is supported by two metal groove contact bearings. A Maxon HEDL5540 encoder
with 500 counts/turn is mounted on the motor to control the angular velocity of the cylinder. This
optical encoder is preferred over a tachometer because we want to be able to control the
deposition position, not just the angular velocity. For data acquisition and interfacing with the
motor and encoder, a TU/e Microgiant is used.
4.7: Translation axis
The translating part in the cylinder spinner design will be mounted on a NSK Monocarrier ball
screw actuator (type MCM05-020-H05K) with a stroke of 200 mm, ball screw lead of 5 mm,
repeatability of 10 m and backlash < 20 m. The ball screw is connected to a Maxon RE30 (type
268219) electromotor with ceramic gear (Maxon, GP32C) via another WM Berg bellow coupling.
A Maxon HEDL5540 encoder with 500 counts/turn is used as sensor. For data acquisition and
interfacing with the motor and encoder, the same TU/e Microgiant as for rotation is used. As
software we employ Matlab Simulink.
4.8: Realisation
The cylinder spinner design was built in Mechanical Engineerings departmental workshop.
Images of the realized design are presented below. In Fig. 28, the stationary part is shown with
the main frame in black PVC. The beige PEEK beam that is mounted to the frame is the electrode
arm. The electrode is made from brass and has a diameter of 0.6 mm and length of 9.5 mm. The

30

matte, glass-like PC beam above it is the nozzle arm. The brass nozzle itself is on the outer edge
on the right. The Teflon polymer transport tube is visible, coming out of the nozzle. The vertical
position of the nozzle arm can be adjusted to change the nozzle-collector and nozzle-electrode
distances. The spindle, carriage, motor and encoder for the spindle axis are also visible in this
photo, but these belong to the translating part which is depicted in Fig. 29.

Figure 28: Stationary part


The translating part consists of an U-shaped frame on which the glass cylinder is mounted. The
cylinder is held up by a large bearing on the left side, which is mounted in a vertical stand, and
the black PVC plug on the right side. The plug is connected to the rotation motor and encoder
which are housed in the black box on the right side of the picture.
The assembled spinner, where the translating part has been mounted on the carriage, can be
seen in Fig. 30. A back-side view of the spinner is shown in Fig. 31. The three wired protrusions
with orange tags at the bottom of the image are the homing switch on the left (marked with zero)
and the two end stops (marked with one and two). More information on the elements can be
found in the next section. In Fig. 32, the spinner is placed in the electrospinning cabin. The
infusion pump is located left of the cabin while the amplifiers and control hardware are located
right of the cabin.

31

Figure 29: Translating part

Figure 30: Electrospinner (front view)

32

Figure 31: Electrospinner (back view)

Figure 32: Electrospinner placed in cabin

33

4.9: End stops, homing strategy, endpoint detection


As described before, the cylinder spinner consists of two parts: a rotating cylinder and a
translating slide. The cylinder is mounted on top of the carriage of the slide. A long, u-shaped
cover is also mounted on the carriage of the ball screw actuator to shield off the slides ball screw
below and prevent it from collecting polymer strands.
The stationary support of the cylinder is outfitted with two Crouzet microswitches which are
placed at each extremity of the slide. These limit points of the slides travel are marked as A and
B in Fig. 33.
A pin protrudes from the cover and can come into contact with a switch. The switches are wired in
such a way that they cut the current to the translation electromotor when one comes into contact
with the pin. As such, they act as end stops and provide mechanical safety.

Figure 33: End stops


It is practical to have a homing procedure to make sure that electrospinning always starts from a
well-defined position and yields a reproducible result. Also, we want to maximize the distance
over which we can electrospin.
There are several methods to home the cylinder spinner. Lets assume we want to home to
position A, and then do spinning while the slide moves from A to B. Since we know the direction
of movement from the encoder data, one way of homing is to move towards and touch end stop 1.
There is a problem with this approach however since once the slide runs into an end stop, any
motor current is interrupted and thus the user is required to manually remove the slide from its
locked position.
Another strategy is to add an additional microswitch as reference point. The next step is then to
choose the location of this reference point. It is possible to place the switch in the middle between
the endpoints of the slide. The problem with this, however, is that it is possible the spinner is in a
position just past the midpoint on the right side when we want to spin from position B.
The best solution is to move the spinner in one set direction upon initialization, i.e. towards A,
and place the reference point just in front of the associated end stop. With this set up, just a
single microswitch is required for homing. This solution was implemented in the electrospinner
design (see Figs. 31 and 34).

Figure 34: Bottom view of endstops (left) and homing switch

34

The current spindle position of the spinner is logged by the motion control and this software shuts
the movement down once the endpoint of the slide is reached.
4.9: Control design
4.9.1: System identification

Phase [deg]

Magnitude [dB]

To enable cylinder motion with high position accuracy, controllers will need to be developed.
Frequency response function measurements were done for both axes to get a good view of
system dynamics. The FRF of the translation axis (spindle) is shown in Fig. 35. A constant
velocity of 1.5 rad/s was supplied as reference. This corresponds to a constant movement of the
spindle of 1.2 mm/s (see Paragraph 4.10). A chirp signal with a decreasing frequency from 2000
Hz to 1 Hz was used as noise signal. The chirp signal resulted in better coherence than a
standard Gaussian noise signal over a larger range of frequencies. The response was measured
for 100 s with a sampling frequency of 4000 Hz.
100
0
-100
-200
0
10
200

10

10

10

-200
0
10
1
Coherence [-]

10

10

10

10

10

0.5

0
0
10

10

10
Frequency [Hz]

10

10

Figure 35: Plant FRF for spindle (fs = 4000 Hz)


The magnitude plot of the FRF shows a slope of -2, which corresponds with a simple moving
mass. In the phase plot we see that delay is present in the system. This delay was modeled with
the following transfer function:

H ( j ) = e jTd

(4.7)

where Td is an aggregate of all effects that contribute to delay, such as discretization and
computation time. Fitting this model on the phase loss yields a delay of 0.65 ms.

35

Magnitude [dB]
Phase [deg]

50
0
-50
-100
0
10
200

10

10

10

-200
0
10
1
Coherence [-]

10

10

10

10

10

0.5

0
0
10

10

10
Frequency [Hz]

10

10

Figure 36: Plant FRF for cylinder (fs = 4000 Hz)


The FRF of the rotation axis (cylinder) is shown in Fig. 36. Going from low frequency to high
frequency, we see a -2 slope, an anti-resonance at 55 Hz, a resonance at 600 Hz and finally
again a -2 slope. A sine wave with frequency of 0.1 Hz and amplitude of 12 rad was supplied
as reference, while a white noise signal with variance of 0.5 was used as noise signal. The
response was measured for 60 s with a sampling frequency of 4000 Hz. A similar fitting
procedure as before yields a delay of 0.80 ms.
4.9.2: Inter-axis disturbances
To see whether movement of one axis registers on the encoders of the other axis and vice versa,
a quick experiment was performed. The same reference signals as in the previous section were
supplied. First, a reference was supplied to the spindle and the cylinder encoders were checked.
Thereafter, a reference was supplied to the cylinder and the spindle encoders were checked. No
inter-axis disturbances were measured. This shows that both axes can operate independently.
4.9.3: GUI and real-time control
A real-time motion controller has been developed with Matlab Simulink. This controller consists of
a graphical user interface (GUI) and real-time code which is generated from a Simulink model.
The GUI is shown in Fig. 37. With this GUI, the user can independently start the translating and
rotating axis, perform a homing procedure and stop the spinner.

36

Figure 37: GUI


4.9.4: Feedback control
Since we want to be able to control where on the cylinder a fiber is deposited, position control will
be implemented for both axes.
First, a feedback controller will be designed for the spindle. As a starting point, a desired
bandwidth of 30 Hz was chosen. By analyzing the open-loop, we notice that the system needs
phase. Therefore, a lead-filter is required (K = 24, z = 30/3 Hz, p = 90 Hz). Furthermore, to
remove steady-state errors, a weak integrator (z = 6 Hz) needs to be implemented. Finally, a lowpass filter (p = 300 Hz) is necessary to reduce the influence of measurement noise.
Secondly, a feedback controller will be designed for the cylinder. As a starting point, a desired
bandwidth of 10 Hz was chosen. By analyzing the open-loop, we notice that the system needs
phase. Therefore, a lead-filter is required (K = 1.2, z = 10/3 Hz, p = 30 Hz). From the FRF, it is
determined that it is desirable to also include a notch to combat the effects of the resonance at
600 Hz and a low-pass filter to reduce measurement noise influences. However, stable
controllers turned out to be unstable after implementation. Therefore, as controller, the before
mentioned lead-filter was used.
An overview of performance is shown in the following table:
Table 7: Performance for both axes
Axis
Bandwidth [Hz] Modulus margin [dB]

Phase margin []

Gain margin [dB]

Spindle
Cylinder

36.5
95.7

9.9
11.3

49.7
3.7

6.0
3.1

Since the spindle will be operated with real-time control that specifies and changes a seconddegree setpoint on-the-fly, feedforward control will not be implemented. The complete control
scheme is shown in Fig. 38.
To test the system, suitable references need to be supplied. A spacing of 100 m was selected
4

as target. This target can be achieved for x& = 8 10 m/s and V = 1 m/s ( = 50 rad/s). In Fig.
39, reference signals r1 and r2 are shown for the spindle and cylinder axis respectively which are
necessary to achieve this target. The homing procedure takes up the first 50 s of the reference.

37

Then, the spinning procedure starts. For r1, a constant velocity of x& = 8 10 m/s is supplied. For
r2, a smooth third order reference is supplied that accelerates for 100 s until it reaches V = 1 m/s.

7
e1

6
r1

5
y1

8
u1
y1 [rad]

e1

r1

u1

Spindle Ctrl

stop1

u1 [V]

stop1

Spindle Ref
y2 [rad]

start

StartRef3

Ref3

acc
vel
pos

e2

Subsystem1

u2

Cylinder Ctrl
2
r2

stop2

u2 [V]
homing [-]

stop2
SystemIO

3
e2

4
u2
1
y2

Figure 38: Simulink control scheme


The associated error signals in time domain are shown in Fig. 40. The position error of the
spindle e1 is roughly 5 m in the spinning interval. The position error of the cylinder e2 reaches a
steady state value of 1 rad at 150 s. This value is unsatisfactory, but cannot be improved at time
of writing.
0.1

r1 [m]

0.05
0
-0.05
-0.1

50

50

100

150

100

150

2500

r2 [rad]

2000
1500
1000
500
0

t [s]

Figure 39: Reference trajectory for s = 100 m

38

-6

10

x 10

e1 [m]

8
6
4
2
50

60

70

80

90

100

110

120

130

140

150

60

70

80

90

100
t [s]

110

120

130

140

150

0.9

e2 [rad]

1.5

0.5

0
50

Figure 40: Measured error signals (time domain)


PSD of e

-40
-50

Power/frequency (dB/Hz)

-60
-70
-80
-90
-100
-110
-120

0.1

0.2

0.3

0.4
0.5
0.6
Frequency (kHz)

0.7

0.8

Figure 41: Measured error signal e1 (frequency domain)

39

PSD of e2
0
-10

Power/frequency (dB/Hz)

-20
-30
-40
-50
-60
-70
-80
-90
-100

0.1

0.2

0.3

0.4
0.5
0.6
Frequency (kHz)

0.7

0.8

0.9

Figure 42: Measured error signal e2 (frequency domain)


To learn more about the error signals, a frequency analysis was performed. The results are
shown in Figs. 41 and 42. The results can be explained by taking the reference trajectories into
account. The references have no high-frequency content and will therefore not excite the system
at high frequencies. Therefore, only errors with low frequencies are expected. This is also what
follows from the figures.
4.10: Spacing error
Quadrature encoders are used as position sensors. Encoders for both axes have a resolution of
500 counts/revolution. The encoder of the spindle is connected to the motor via a gearbox with a
reduction of 23/4:1. The spindle has a lead of 5 mm, thus the translating part moves 5 mm for
every revolution. One count of the spindle encoder then corresponds with:

2
= 5.46 10 4 rad
500 4 23 / 4

(4.8)

0.005m / rev
= 4.35 10 7 m
500 4 23 / 4

(4.9)

The cylinder encoder is directly coupled to the encoder and one count thus corresponds with:

2
= 0.0031rad
500 4

(4.10)

With this information, a measured constant position error e in [rad] can be related to the error
along the associated axis. The error in the spacing can then also be calculated.

40

We define the spacing error s as the difference between the desired spacing s and the realized
spacing s :

s = s s

(4.11)

The desired spacing can be calculated from the desired translation velocity x& and the realized
collecting speed V :

s=

2Rx&
V

(4.12)

The realized spacing can be calculated from the realized translation velocity x& and the realized
collecting speed

s =

2Rx&
V

V :
(4.13)

As the derivatives of the positions of the translation and rotation axes were very noisy, it was not
possible to determine the realized spacing error at the time of writing.

41

Chapter 5: Post-design experiments


Now that the cylinder spinner design has been realized, experiments can be performed to review
its performance. In Paragraph 5.1, deposition experiments are performed on the stationary
cylinder to determine whether focused deposition occurs testing a wide range of spinning
parameters. Thereafter, in Paragraph 5.2, it is checked to see if the electric field disturbs the
sensors and electromotors. A number of problems with the setup manifest themselves during
testing. In Paragraphs 5.3 and 5.4, the causes of these problems are analyzed and some
solutions are presented.
5.1: Stationary deposition experiments on glass cylinder
5.1.1: Experiments
Now that the cylinder spinner is realized, deposition experiments can be performed with it. The
goal of these experiments is to determine whether focused deposition occurs for a wide range of
spinning parameters. These initial experiments will be performed with a stationary cylinder. PEO
is used as polymer solution. A mylar sheet is wrapped around the cylinder to collect the fiber.
Fourteen experiments will be executed, varying: the applied voltage V in a range from 12 to 25 kV,
the feed rate f from 10 to 18 l/min and d the vertical distance between nozzle tip and collecting
material from 8 to 13 cm.
5.1.2: Results
All mylar films showed similar random depositions. In Fig. 43, a representative result is shown.
Two black lines at the top and right edges of the cylinder were added to the sample to indicate
the location of the needle electrode. The electrode was placed at the interception point of the
black lines in the center of the image. The deposition resembles that of a plate electrode, but it
was checked that there was no contact between the cylinder and electrode. Note that there is a
gap in the deposition at the bottom of the image, because this was the location of a piece of tape
to stitch both edges of the mylar sheet together.
From tuning V and keeping other parameters constant we learn that the deposition for low V is
less concentrated and less dense than for high V. The changes are marginal, though, and all
results are very similar to Fig. 43. An interesting observation was that for V > 22 kV the jet splits
in multiple sub-jets immediately after leaving the nozzle tip.
Tuning f and d did not enhance the focus of the deposition.
It had been expected that a well-defined spot of deposition would be formed, but this is not what
is observed. Clearly, this is a significant problem. Since spinning parameters were varied over a
wide range, it is highly likely that the lack of sharp focusing is due to the construction rather than
operating conditions. In Paragraph 5.3, a number of experiments will be described to determine
the cause of this problem.
5.2: Testing with motion
As a first motion test, the cylinder spinner was supplied with standard position references for the
rotation and translation axes. Simultaneously, the realized positions and errors were recorded.
Then, the electric field was powered up with an applied voltage of 10 kV and the same
trajectories were supplied. No significant differences in the position errors of both axes were
observed. The test was repeated for 15, 20 and 25 kV with identical results. It was therefore
concluded that the electric field has no influence on the encoders and motors and that the
measures employed to shield off the electric components are sound.

42

During further testing it was discovered that the current hardware of the cylinder spinner is not
capable of reaching the required collection speed of 8 m/s. The upper boundary is currently 1 m/s.
This limitation is due to mechanical problems in the rotational axis of the setup. Causes are
expected to be: the out of roundness of the cylinder (measured: 0.3 mm), misalignment between
cylinder axis and rotation motor axis, and significant friction in the bearing.

Figure 43: Representative result of spinning on mylar wrapped around glass cylinder

5.3: Troubleshooting
To locate the cause of the focusing problem, as systematic approach will be undertaken using the
grounded needle electrode setup as reference. Elements of the setup are exchanged with those
of the cylinder spinner and the following combinations are investigated:
1. Grounded needle electrode setup, described in Chapter 3, modified so that the nozzle is
just an injection needle protruding from a charged horizontal copper plate.
2. Same as 1, but with the cylinder spinners nozzle arm.
3. Same as 1, but with the cylinder spinners electrode arm.
4. Cylinder spinner setup with mylar sheet as collector.
5. Cylinder spinner setup with glass cylinder (t = 2.5 mm) as collector.
The results of experiments with these combinations will be compared for the same spinning
parameters. Note that all results have been repeated several times and the images of
representative results are presented below.

43

Comparing results of 1 to 2:
In Fig. 44a, the result with combination 1 (grounded needle + nozzle out of plate + mylar) is
shown, while in Fig. 44b combination 2 (grounded needle + nozzle-arm + mylar) is represented.
From the results it is learned that the nozzle arm of the cylinder spinner does not hamper
focusing. On the contrary, deposition seems to be more aggressively focused and resembles
writing.

Figure 44: Comparing deposition of:


(a) Combination 1. (b) Combination 2.
Comparing results of 1 to 3:
In Fig. 45a, the result with combination 1 (grounded needle + nozzle out of plate + mylar) is
shown, while in Fig. 45b combination 3 (electrode-arm + nozzle out of plate + mylar) is
represented.

Figure 45: Comparing deposition of:


(a) Combination 1. (b) Combination 3.

44

Both figures show a random deposition although this deposition is denser in Fig. 45a. In the right
figure, two big white drops are present. The one in the center of the image was caused by a drop
deposited after the electric field was switched off and should therefore be ignored. It is concluded
that using the cylinder spinners electrode arm gives similar results, although less concentrated.
Comparing results of 2 with 4:
In Fig. 46a, the result with combination 2 (grounded needle + nozzle-arm + mylar) is shown, while
in Fig. 46b combination 4 (electrode-arm + nozzle-arm + mylar) is represented. From this figure it
can be observed that both depositions consist of a writing-like deposition with some thick fibers
produced halfway through the experiment.

Figure 46: Comparing deposition of:


(a) Combination 2. (b) Combination 4.
It is logical to conclude that writing is enabled by the nozzle-arm.
Comparing results of 4 with 5:

Figure 47: Comparing deposition with electrospinning setup on:


(a) Combination 4. (b) Combination 5.

45

In Fig. 47a, the result with combination 4 (electrode-arm + nozzle-arm + mylar) is shown, while in
Fig. 47b combination 5 (electrode-arm + nozzle-arm + glass) is represented. When switching
from the thin mylar to the relatively thick glass as collector, the deposition type changes from
focused to random.
From the experiments in this Paragraph it can be concluded that the electrostatic properties of the
nozzle and electrode arms are satisfactory. The glass cylinder is the element that prevents proper
focusing.
5.4: Stationary deposition experiments on PET
Through experiments it was discovered that the glass cylinder with a thickness of 2.5 mm
prevents proper focusing of polymer fibers. While one can produce a glass cylinder with a smaller
wall thickness, one has to take the operating conditions into account. The rotation axis of the
cylinder spinner operates at high angular velocities and therefore a thinner glass tube might be
problematic. Aspects like ease-of-handling, safety and durability could become issues. In
electrospinning experiments we wrap a thin sheet of collecting material around the cylinder on
which the deposition takes place. A thin glass tube breaks easily and special care must be taken
when mounting the collecting material. As mentioned before, high angular velocities are used and
designing a setup that does not vibrate during motion and does not lead to failure of the glass is
nontrivial.
Rather than installing a new cylinder with smaller wall thickness, it was deemed more prudent to
investigate the possibility of using a different cylinder material. Polyethylene terephthalate (PET)
was selected because it cannot break, is easy to process, readily available and essentially the
same material as mylar.
5.4.1: Experiments
Cylindrical PET samples with a diameter of 8.5 cm, length of 9.5 cm and wall thickness of
0.25 mm were obtained from the departmental workshop. For each experiment, a new PET
sample will be mounted in the cylinder spinner setup to replace the glass cylinder. An airgap of 10
mm between PET collector and electrode is established. PEO solution will be electrospun on the
samples using the following spinning parameters:
Table 8: Spinning parameters for PET deposition experiments
V [kV]
f [l/min]
t [s]
D [cm]

a [mm]

17

10

18

60

11

5.4.2: Results
It was discovered that it is relatively easy to electrospin on PET cylinders using the parameters in
the previous section. Even with an airgap of 10 mm, which is significantly larger than the airgaps
used in this research project for mylar and glass, focusing is very good. All three experiments
show similar results. Here, one representative result will be presented (see Fig. 48).
Again, black lines were added to the sample to indicate the location of the needle electrode.
In the first 20 seconds of the experiment, the deposition process resembles the writing-like variety
we are accustomed to from other experiments where the cylinder spinners nozzle arm is used.
This deposition can be recognized as the hazy spot of fibers in the centre of the image. After this
time has lapsed, the deposition becomes less focused. The polymer jet seems to lash from the
centre of the collector outwards. During this movement, the majority of the polymer seems to slide
along the already established or solidified jet while the deposition point traverses radially away

46

from the deposition point. This is not unlike other experiments where the same phenomenon has
been observed. The associated deposition can be seen in the center-left part of the image and
consists of thicker fibers.

Figure 48: Representative result of spinning on a PET cylinder


It is postulated that this different deposition is due to the fact that the needle electrode has been
shielded off by the writing-like deposition that has happened earlier, but further tests are
necessary to confirm this hypothesis. When a rotating cylinder is used instead of a stationary one,
the deposited charge is moved away from the deposition point and shielding is no longer an issue.
PET offers significantly better focusing and is therefore a viable alternative for glass as cylinder
material.

47

Conclusion and recommendations


In this report, a new position-controlled electrospinner was designed, constructed and tested. The
design was based on electrostatics and the results of a set of pre-design experiments with PEO
and PCL. A number of conclusions can be drawn from these experiments:

Although deposition mechanisms for the grounded plate and needle electrodes on mylar
and glass are different, the deposition looks similar.
Mylar writing samples were created with PEO and PCL. Fibers of both polymers have a
rectangular cross section. The PEO fibers had a height of 380 nm and a width of 8 m,
while the PCL fibers had a height of 14 m and a width of 27 m.
It was qualitatively determined for glass and polycarbonate that the influence of collector
thickness does indeed play a role in the amount of deposition that takes place.
No apparent visible difference was detected between deposition on mylar in direct
contact with a needle electrode and with an airgap in between. The airgap did not prevent
or hinder deposition.

Two problems popped up:


1. Focusing did not occur when using a glass cylinder with thickness of 2.5 mm.
2. The desired collecting speed of 8 m/s could not be reached.
Through a number of post-design experiments, it was found that:

The lack of focusing was caused by the relatively high thickness of the glass cylinder.
Changing parameters V, f, d had no effect.
The nozzle arm of the cylinder spinner enables better focusing than a nozzle protruding
from a horizontal charged plate.
A PET cylinder is a good alternative to the glass cylinder currently installed in the setup.

There are a few recommendations for further research:

It is suggested to redesign the rotation axis so that the required collecting speed can be
attained.
Another solution is to use a different polymer that requires a lower collecting speed than
PEO.
Better position control might be possible by implementing feedforward control.
The glass cylinder can be replaced with a PET cylinder for better focusing.
The current electronics that are used to operate the cylinder spinner are rather bulky. It
might be practical to rearrange them in a more compact form.

48

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