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AFM Characterisation of

Technical Fibres
Q.F. WEI*
Southern Yangtze University
Wuxi 214063, PR China

X.Q. WANG
Anhui University of Technology & Science
Wuhu 241000, PR China

ABSTRACT: Technical fibres are designed and produced to create microstructures


that give the fibre product its characteristic properties. The use of new tools is of
importance in fundamental and practical research and development of versatile
technical fibres for a variety of applications. This paper highlights the methodo-
logical approaches to exploring the nanostructures, properties, and dynamics of
surfaces and interfaces of technical fibres using Atomic Force Microscopy (AFM).
The examples presented include structure characteristics of nanofibre materials,
nanostructure and properties of fibre surfaces, nanoscale level interactions at fibre
interfaces, and dynamic nanostructure evolution of fibre surfaces under different
conditions. In these areas, AFM is shown to be a useful and versatile tool to study
nanostructures, to probe surface and interface properties, or to investigate the
dynamic process at fibre surfaces and interfaces. AFM provides powerful tools for
nondestructive characterisation of technical fibres.

KEY WORDS: technical fibres, AFM, nanostructure, surface, interface.

INTRODUCTION

increasingly developed and used in many


T ECHNICAL FIBRES ARE
industries [1]. Ever-expanding demands are driving the technological
innovations in creating distinct, well-defined structures of fibres on the

*Author to whom correspondence should be addressed. E-mail: qufu_wei@sina.com

JOURNAL OF INDUSTRIAL TEXTILES, Vol. 34, No. 1July 2004 51


1528-0837/04/01 005110 $10.00/0 DOI: 10.1177/1528083704046569
2004 Sage Publications
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52 Q.F. WEI AND X.Q. WANG

nanometer scale. The technical properties of these fibres closely depend on


the molecular structures of their surfaces and interfaces. Consequently, the
control of technical properties requires the characterisation and controlled
assembly of these nanostructures at their surfaces and interfaces.
It is well known that the characteristics of fibre surface can affect wetting,
stiffness, strength, dyeing, and other performance properties and these
effects are also closely related to production optimization and product
properties [2]. In many applications of technical fibres, interfaces are also
formed between two phases of either the same or different materials.
Understanding of fibre interface behaviours are of importance in developing
textile composites and other high performance products [3]. Studies under
dynamic conditions will give us new insight into the kinetics of structure
formation, rearrangement, and breakdown that are important for the
processing and product development of technical fibres and fibrous
products as well as other structured products.
Microscopy technology provides the tools for describing how a particular
structure is engineered, and, therefore, how it relates to the properties of the
product. Approaches in which microscopy methods are combined with
other techniques can promote the understanding of the structural role of
individual fibres and their effect on the overall microstructure of the fibre
products [4]. New developments within microscopy, such as Environmental
Scanning Electron Microscopy (ESEM) [5] and Atomic Force Microscopy
(AFM), open up new avenues for technical fibre research and development.
This article highlights AFM techniques and approaches to the study of
the nanostructures of technical fibres.

AFM

The atomic force microscope (AFM), developed in the mid 1980s, uses
a sharp probe to magnify surface features. AFM is being used to probe
materials including thin and thick film coatings, ceramics, composites,
glasses, synthetic and biological membranes, metals, polymers, and
semiconductors [6].
This microscope operates by measuring attractive or repulsive forces
between a tip and the specimen. The AFM uses a probe that has a nano-size
tip mounted on a flexible cantilever as shown in Figure 1. The tip is slowly
scanned across the surface of a specimen. The force between the atoms
on the surface of the scanned material and those on the scanning tip cause
the tip to deflect. The magnitude of the deflection depends on the separation
between the surface atoms and the tip atoms and on the atomic forces
between them. This deflection can be recorded by using a laser focused

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AFM Characterization of Technical Fibers 53

FIGURE 1. Atomic force microscopy.

on the top of the cantilever and reflected onto photodetectors. The photo-
detector signals are used to map the surface characteristics of specimens
with resolutions down to the nanoscales. Piezoelectric transducers control
the lateral and vertical movements of the tip and a feedback loop that
produces voltage differences proportional to the movement.
There are three scan modes for AFM:
(1) Contact Mode AFM
(2) Noncontact AFM
(3) Tapping Mode AFM.
In contact mode, the tip scans the specimen in close contact with the
surface of the material. The repulsive force on the tip is set by pushing the
cantilever against the specimens surface with a piezoelectric positioning
element. The deflection of the cantilever is measured and the AFM images
are created.
In noncontact mode, the scanning tip hovers 50150 A above the speci-
mens surface. The attractive forces acting between the tip and the specimen
are measured, and topographic images are constructed by scanning the tip
above the surface.
Tapping mode imaging is implemented in ambient air by oscillating the
cantilever assembly at its resonant frequency (often hundreds of kilohertz)
using a piezoelectric crystal. The piezo motion causes the cantilever to
oscillate when the tip is not in contact with the surface of a material. The
oscillating tip is then moved toward the surface until it begins to tap the
surface. During scanning, the vertically oscillating tip alternately contacts
the surface and lifts off, generally at a frequency of 50,000500,000 cycles
per second. As the oscillating cantilever begins to intermittently contact the
surface, the cantilever oscillation is reduced due to energy loss caused by
the tip contacting the surface. The reduction in oscillation amplitude is used
to measure the surface characteristics.

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54 Q.F. WEI AND X.Q. WANG

The AFM used in this work was a Topometrix TMX 2000. The images
were scanned in contact mode AFM with a silicon nitride cantilever. All
images were obtained at ambient conditions. The scanner head had a
maximum scan range in x-, y-, z-direction of 100  100  8 m3, respectively.

AFM CHARACTERISATION OF FIBRE NANOSTRUCTURES

The characterisation of the nanostructures of technical fibres is of


importance in understanding their performance and structureproperty
relationship. The characterisation of surfaces and interfaces of individual
fibres and fibrous assemblies is of special interest to many scientists and
engineers as these determine the properties of the products made from
the materials. There are different ways in which AFM can be used to
characterize fibre surfaces and interfaces.

Structures of Nanofibres

Nanofibre generally refers to a fibre with a diameter less than 1000 nm.
Polymer nanofibres can be made using the electrospinning process [7].
Polymer nanofibres are used in a variety of fields, including filtration,
biomedical and composites applications.
One of the most important quantities related with electrospun nanofibres
is the fibre diameter and fibre structure. Since nanofibres are produced from
polymer solutions, the fibre diameters and structures will depend mainly
on the settings of the electrospinning process. The AFM images of the
electrospun polyamide 6 are shown in Figure 2. The fibres were spun from
the polyamide 6 solution with a concentration of 10wt.%, prepared by
dissolving the polymer in formic acid. The polymer solution was electrospun
at 15 kV from a syringe and the spun fibres were collected on a grounded
aluminum foil.
The image in Figure 2(a) shows the three-dimensional fibrous web,
consisting of fibres with diameters ranging from less than 300 to over
1000 nm. The fibres are randomly oriented and the pores with varying sizes
are formed. The image also indicates that the diameter is uneven along an
individual fibre. Figure 2(b) is an AFM image showing the nanofibres laid
onto an ordinary nonwoven substrate. The nanofibres form a network
with much smaller pores covering the bigger pores among the normal
nonwoven fibres. The nonwoven substrate provides mechanical properties
the material needs, while the nanofibres can improve the performance of
the web.

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AFM Characterization of Technical Fibers 55

FIGURE 2. The AFM images of nanofibers: (a) nanofibers and (b) nanofibers laid on
nonwoven substrate.

Surface Characterisation of Technical Fibres

The AFM is able to physically examine technical fibre surfaces without a


conductive coating. Fibre surfaces play an important role in determining the
fibre properties. The surface structures of technical fibres can be customized
to meet the needs of different technological applications depending on the
understanding of the relations between the production settings and the
surface morphology development.
The polypropylene fibres were used as an example in the surface char-
acterization by AFM. The polypropylene fibres were spun on a Labspin

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56 Q.F. WEI AND X.Q. WANG

(a)

(b)
FIGURE 3. The AFM images of polypropylene fiber surface: (a) as-spun fiber and (b)
drawn fiber.

extruder (Extrusion System Limited (ESL) using the HF445J B2-9037


polypropylene chips supplied by Borealis.
As illustrated in Figure 3(a), the deformed spherulites can be seen on
the surface of the as-spun fibres. The transformation from a spherulitic
morphology to a fibrillar structure was found as the fibres were stretched as
shown in Figure 3(b). It can also be seen from Figure 3(b) that these
nanofibrils have varying diameters.

Interface Characterisation of Technical Fibres

The characteristics of interfaces are usually different from those of the


bulk phase(s). The goal of fibre interface studies is to facilitate the manu-
facture of technological fibres with optimized properties on the basis of the

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AFM Characterization of Technical Fibers 57

comprehensive understanding of interfacial behaviours of technical fibres


and their resulting influence on material processes.
The AFM is a nondestructive image tool; therefore it is an important tool
for the interfacial studies of technical fibres.
The AFM images in Figure 4 show the interfaces between aerosol
particles and the fibre filter. Aerosols from the domestic atmosphere were
sucked through a PET nonwoven filter for 24 h. As air passes through the
fibres they attract and hold particles on their surfaces. Figure 4(a) is an
AFM image of aerosols captured on the PET electret filter. The particles
with a square shape are probably sediments from the walls or ceilings.

(a)

(b)
FIGURE 4. The AFM images of interfaces: (a) aerosol particles on PET electret filter
and (b) aerosol particles on PET filter.

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58 Q.F. WEI AND X.Q. WANG

Particle-size distributions can be easily obtained either from manual


analysis of the three-dimensional data set provided by AFM or through
the use of an image analysis. The nanosized particles can be seen on
the fibre surface, which are perhaps fly ash or fine dusts. The particle
on the left is a fibre-like dust and may be a short fibre. Figure 4(b) is
another image of aerosol particles collected on the same PET non-electret
nonwoven filter. In this case, since the particles were captured without
electrostatic force, there are much less nanosized particles captured on the
fibre surface.

Dynamic Characterisation

The atomic force microscope is also capable of examining dynamic


changes under varying conditions. The ability to follow dynamic events will
give new insight into the kinetics of structure formation, rearrangement, and
breakdown that are important for the processing and product development
of technical fibres and fibrous products as well as other structured products.
Structure engineering can drive the development of new processes yielding
tailor-made structures to give products the desired properties.
The series of AFM images in Figure 5 demonstrate the dynamic changes
that occurred on the fibre surface by plasma treatment. The untreated PP
surface shows a smooth texture with fibre-like structures probably induced
by the dawning of the fibre as shown in Figure 5(a). Figure 5(b) shows the
PP fibre surface treated with O2 plasma for 3 min at a power of 100 W and
airflow of 0.1 L/min. The sample treated has lost its original surface features
and presents aggregates with varying sizes on the fibre surface. Its surface
roughness has been greatly increased by the O2 plasma treatment for 5 min
at the same power and airflow. The nanoporous surface was formed by the
prolonged treatment as shown in Figure 5(c).
The AFM images indicate that the nanostructured surface can be created
by the plasma treatment. Different structures can be formed by the different
settings of the treatment. The defined surface structures may be created for a
special need.

CONCLUSIONS

This study has explored the use of the Atomic Force Microscopy (AFM)
for the characterisation of technical fibres under varying conditions. The
ESEM provides a new and powerful approach to the examination of the
nanostructures of technical fibres. The potential use of the AFM in technical
fibre research and development is promising and significant.

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AFM Characterization of Technical Fibers 59

(a)

(b)

(c)
FIGURE 5. The AFM images of dynamic process: (a) untreated PP fiber; (b) plasma
treated PP fiber (3 min) and (c) plasma treated PP fiber (5 min).

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