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Electron microscope studies of textile fibres

and materials*
J. W. S. Hearle
Department of Textile Technology, University of Manchester
Institute of Science and Technology, Manchester M60 1QD, UK

and S. C. Simmens
Shirley Institute, Didsbury, Manchester, UK
(Received 1 December 1972)

INTRODUCTION material wholly or partly encasing the fibre or to find
some means of breaking open a replicating skin around
Historically, the examination of fibres occurred early in a fibre. Sectioning also has its special difficulties with
the use of electron microscopes. Two of the first seven
fine fibres.
commercial RCA electron microscopes to come to this At lower magnifications, the study of fibre assemblies,
country under lend-lease in 1942, went to the Shirley textile yarns and fabrics, is a use of scanning electron
Institute (then the British Cotton Industry Research
microscopy which has many special problems and
Association) and the Textile Physics Laboratory of the
applications. Direct electron microscopy has no applica-
University of Leeds. In the 1950s, Chapman et alA, 2,
tion to the study of fibre assemblies.
as part of a study of fibre friction, developed the use of
In this review, we shall first outline the general range
the reflection mode of a direct electron microscopet to of techniques and applications for electron microscopy
study fibre surfaces--a technique now superseded by in textile and fibre laboratories, describing in more
scanning electron microscopy. Later, the first scanning
detail some recent techniques; and, second, comment on
electron microscope to be used in an applications labora-
two topics of continuing interest--the nature of the
tory was made at Cambridge University and sent to the
fine structure, where direct electron microscopy gives
Pulp and Paper Research Institute of Canada; and two
information, and fibre fractography, where scanning
of the first three commercial instruments went to textile
electron microscopy is important.
fibre laboratories. However, despite this priority, it
remains true that the electron microscopy of individual
textile fibres is really just a special case of the electron USE OF ELECTRON MICROSCOPES IN TEXTILE
microscopy of polymer materials, providing also, in LABORATORIES
natural fibres, a link to biological studies, though without A direct electron microscope is a necessary tool in any
the severe problems associated with the collapse of cells laboratory concerned with experimental studies of fibre
on drying. structure or fibre surfaces, and is found in the research
Some special features do arise from the size and shape laboratories of the major fibre producers and in coopera-
of fibres, which, are by definition, long fine units of tive and academic laboratories. The scanning electron
matter. The lateral dimensions of fibres (around 10/zm) microscope, and indeed the optical microscope, is a
are only a little greater than the wavelength of light, and complementary instrument for fibre studies, and has
consequently even comparatively gross features of fibre also greatly increased the range of textile problems which
structure, below about a tenth of a fibre diameter, can be studied by electron microscopy (e.m.): the appli-
cannot be examined effectively by optical microscopy. In cations to textile fibres have been pioneered by Billica's
practice, the restricted depth of focus is as severe a group in du Pont (Kinston, North Carolina), Sikorski's
difficulty as the limited resolution. For example, the group at Leeds, and the group at UMIST.
general morphology of fibre fracture surfaces could not However, the heavy utilization of an electron micro-
be clarified until the use of scanning electron microscopy scope of either type in a textile laboratory is partly made
(s.e.m.). up of other applications: the study of additives, such as
In electron microscopy, the fineness and cylindrical starches, pigments, and resins; the study of metal,
shape of fibres cause some difficulties in replication, plastic, or ceramic machine parts; and service work in
because it is necessary either to prevent the replicating completely different fields.
* Presented at the symposium 'Application of electron microscopy
to the study of polymers' on 12 September 1972 as part of the 5th Direct electron microscopy
European Congress on Electron Microscopy (EMCON 72) held a t Table 1 lists those techniques which would be regarded
the University of Manchester. as being in the standard repertoire of a fibre electron
t The term direct electron microscope is used to denote an electron
microscope of the earlier type, often, misleadingly,called a trans- microscope laboratory and indicates the nature of the
mission, conventional, or traditional electron microscope. applications. In this section we briefly consider the

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Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens
Table I Common techniques and applications of direct electron in another way; a piece of fabric can be shadowed and
microscopy to fibres carbon-coated and pressed lightly or even laid on the
Techniques Applications heated polystyrene. When cool the fabric can be stripped,
mechanically or chemically, and the replica fragments
Basic specimen: recovered by dissolving the polystyrene.
Replica of fibre surface* Surface structure (e.g. scales on
wool), roughness, and modifica- In Figure 1, the surface detail on a nylon filament
tion. Surface defects or damage. can be seen at relatively high magnification. This is a
Observation of soiling or foreign replica made in the way described. The feature of interest
objects is the numerous needle shaped crystals of about 200 x 6 nm
Thin transverse section Observation of fibre cross-sec-
(low magnification)* tional shape, and gross structural
size. This fibre was in a fabric that did not bond well
features to a foam laminate; it was found that the use of acid
Whole fibre silhouette* Fibre axial shape dyestuffs followed by a synthetic tanning agent produced
Replica of cut surfacet poor bonding and this was associated with the presence
Replica of peeled surfacet of the crystal detail seen on the fibre surface. This
Replica of fractured surface¢
Mechanical disintegration Contribution to elucidation of fine technique is not unlike that of Scott 5, who used chromium
(blendor)*t structure of fibres instead of carbon, then placing the filament into a
Ultrasonic disintegration*t viscous solution of poly(acrylic acid) and subsequently
Chemical disintegration*¢ stripping chemically or mechanically to leave the chro-
Thin transverse or
longitudinal section (high
mium behind in the poly(acrylic acid) from which it
magnification) was recovered by dissolution of the poly(acrylic acid) in
Other features: hot water.
Enhancement of contrast by In Figure 2, we see this method applied to the surface
shadowing* or staining of a polyester filament--the titanium pigment can be
Dark-field viewing*
Selected area diffraction* Crystal structure or identification seen to be exposed at the fibre surface and suggests how
guides and knitting needles come to be cut by an easily
* In common current use at Shirley Institute deformable polymer substance.
t At high magnification; use s.e.m, for lower magnification Figure 3 shows a fibre surface after etching in a glow
discharge with argon6; this was done to examine the
application of some general laboratory techniques or effect of such treatment on the soiling properties of
day-to-day applications of direct e.m. for which experi- polyester fabric and is a further example of the technique
ence shows that there is a continuing use. As those who of Scott.
work in the field are all too aware, textile fibres are too Although the literature contains numerous papers
big in their entirety for fine structure to be shown up wherein a plastic has been used for replication, our
in transmission electron microscopy, yet they offer experience is that plastic replicas at best give low or
practical difficulties in handling because of their small poor resolution and at worst misleading artifacts;
diameter and chemical nature. However, for a number nowadays better and more reliable pictures can be
of purposes there is in fibres a level of detail not yet obtained by s.e.m. We do, however, find Chippendale's
accessible by other means. technique ~ useful at times (he used Formvar softened
Of the various approaches that can be used to obtain
information many have a very long history of develop-
ment and refinement; but, even so, relative newcomers
to the field, like ourselves, find difficulty in translating
published techniques into reliable routine methods, and
we propose here only to discuss those general techniques
that work for us.
Considering first the surface detail of fibres, replication
is necessary in order to examine this; and the major
problem involved is that, owing to their small diameter,
fibres are liable to be encapsulated by the replication.
Dlugosz a and Ramanthan et aL 4 realized this many
years ago, and applied the principle of first semi-embed-
ding the fibre in some medium such as gelatine or resin
for up to half its depth or thickness; the exposed upper
portion of the fibre was then replicated by a silver/carbon
or similar technique. This method, though having
several steps, works well when one has fibres that are
in a shape or form that can be semi-embedded and it
gives a final resolution as good as any that can be
obtained. In the intervening years since this approach
was introduced other semi-embedding media have been
used. Fibres that can tolerate a temperature around
150°C can be laid on a thin disc of freshly pressed poly-
styrene which is then heated; the fibres sink into the
polystyrene with, fortunately, a contact angle of about
90 °, the depth of embedding being controlled by time Figure 1 Pre-shadowed carbon replica of nylon filament surface
and temperature. Thin discs of polystyrene can be used showing numerous fine dyestuff crystals (S.C.S.)

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Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens

deposit contains much plate-like material and the ED
pattern from this is compatible with a clay deposit.
From Table 1, it can be seen that various techniques
are available for the examination of internal detail in
fibres; the apparently most direct is that of sectioning
and over the years much effort has been expended in
this direction. From the results published it is clear that
useful information about the internal structure of wool,
in particular, and also cotton can be and still is being
obtained; but that with man-made fibres this is not a
profitable line of approach. Mainly this arises from the
difficulties associated with the sectioning of polymers,
and so far there appears to be little information that
cannot be obtained more easily by other means. Consider,
for example, the titanium pigment present in most
polyamide and polyester fibres and about which there is
a continuing need for information as pigment can vary
in size, shape and degree of aggregation. Sectioning may
seem a direct approach but let us look at a different one.
Figure 5 shows a polyester filament etched in a glow-
discharge with argon. It provides an excellent view of the
distribution of the pigment in the fibre, as here the
discharge has been allowed to etch well into the fibre
allowing the pigment particles to stand out. Incidentally
they are now accessible to extraction techniques, if we
want to look at them closely or use ED. This appears
to us a worthwhile approach to the study of pigment
distribution in fibres. It can be further supplemented by
direct examination of the particles (Figure 6); here the
Figure 2 Chromium replica of a polyester filament surface show- yarn was dissolved, the pigment separated out, washed
ing exposed titanium pigment (S.C.S.) and sprayed on to a carbon coated grid.
A further means of opening up the internal structure
of fibres is by mechanical on physical disintegration.
Beating in a blendor device and ultrasonics have been
used, and, as discussed later, we have recently applied
freeze-pressing as a method to break down fibres. The

Figure 3 Chromium replica of polyester filament surface after a
glow discharge treatment (S.C.S.)

with acetone as the primary replicating medium) on
account of the fact that it will often strip a deposit from
a fibre; the deposit finishes up in a carbon replica, and
thus becomes accessible to electron diffraction (ED).
In Figure 4 we have the final carbon replica, from
Chippendale's method, of a cotton fabric containing a Figure 4 Carbon replica (Chippendale technique) illustrating the
deposit. At higher magnifications we can see that the removal of a deposit from cotton fibres (S.C.S.)

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Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens

however, is still much used in a routine way. The choice
of liquid in which the beating is done is of importance:
cotton in white spirit cannot be fibrillated, but cotton in
water readily fibrillates into microfils having a size
around 100A, some of which split at the ends into finer
strands (Figure 7). With prolonged beating, much ultra-
fine fibrillar material, 50 A and less, is obtained. Cotton
beaten in caustic soda passes quickly from microfibrils
of 100A, or less, to an extremely finely divided material.
Internal detail can also be examined by the splitting
and peeling techniques, described by Scott 5, in which a
nick is cut in the fibre surface and then peeled back to
display an internal surface for replication.

Scanning electron microscopy
The usual repertoire for scanning electron microscopy
is given in Table 2, with a list of typical applications. As
in all scanning electron microscopy, the ease of prepara-
tion, the apparent directness (despite the instrumental
indirectness) of observation, and the ease of manipulation
of specimens is a great advantage. The standard pro-
cedure at UMIST would be to take a textile specimen as
provided, stick it to Twinstick previously mounted on the
stub and coated with a thin layer of gold or silver*,
then coat the specimen with gold or silver, and examine
it in the s.e.m, at 5kV. Where fibre ends have to be
examined, the fibre would usually be held between
Sellotape, with 1 mm projecting, and then clamped in a
split stub and coated with gold or silver. There are
Figure 5 Polyester filament strongly etched in a glow discharge circumstances where metal coating is undesirable. An
to show the distribution of the titanium pigment (S.C.S.) antistatic agent such as Duron can be used as an alter-
native; at UMIST we commonly soak the material and

* Silver is suitablefor immediateuse; but gold is used for specimens
which need to be kept for some time,

Figure 6 Titanium pigment extracted from polyester filament
(S.C.S.)

preparation from some fibres made by this method a r e
excellent for ED work; in some respects this form of
disintegration is superior to using a blendor. It does not,
for example, produce so much of the extremely finely
degraded material (flour-like in the micrographs) as the
blendor does. Figure 7 Cotton microfibril showing splitting into finer units
Mechanical disintegration of fibres in a blendor, (s.c.s.)

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Table 2 Common techniques and applications of scanning luminescence can also be used, though care is needed in
electron microscopy to fibres, yarns and fabrics interpretation of results on complicated surfaces, because
the contrast arises both from differential light emission
Techniques Applications
and direction (topographical contrast).
Basic specimen : Low magnification
Direct observation of Assembly structure--arrangement
sample* of fibres in yarns or non-woven SOME SPECIAL TECHNIQUES
fabrics, and yarns in woven or
Cut end (plate method)* knitted fabrics as produced or Swelling and staining
modified The central problem in the use of electron microscopy
Section, moderately
thick (>1/zm)*
to help in understanding fibre structure is to find a
Presence of soil or foreign objects means of showing up structural elements which may be
Disintegration of fibres Identification of fibres in structure present.
(blend distribution, faulty fibres) It has been common practice to stain fibre sections to
Peeling of fibres Observation of damage in textile enhance contrast, e.g. heavy-metal containing substances
products
Thin section such as osmium tetroxide are taken up differentially by
Examination of original, Medium magnification: wool fibres depending on variations in protein composi-
cut or ruptured Fibre shape and form tion. However, the range of techniques is steadily being
surfaces* Fibre surface structure, roughness, expanded. For example, Swift 9 has developed specific
Other features: defects or damage
Reduction of charging Particles on fibre surface stains for particular amino acid residues in hair fibres.
by metal-coating, or Fracture morphology Stains can also be used to show up differences in accessi-
soaking or spraying Gross internal features (cell struc- bility, and for this purpose a mild swelling treatment
with antistat* ture in wool, voids, macrofibrils, etc) may first be given. Ingrain1°, 11 treats cellulose fibres,
Distribution of resins or finishes
Choice of viewing angle (external or internal) location of
such as Ramie, with caustic soda and then phosphotung-
conditions and variations in composition stic acid in order to show up a fibrillar structure.
magnification* A further development has been reported by Billica
Analysis of X-ray et al. 12. A synthetic fibre is swollen in the vapour of
emission High magnification: boiling methyl methacrylate (or some other vinyl mono-
Imaging in X-ray mode Fracture detail
Contribution to elucidation of fibre mer) for about 3 h; polymerization of the monomer
fine structure then occurs over a few days and, finally, the reactive
polymer, which now impregnates the fibre, is stained
* In frequent use at UMIST with osmium tetroxide. In addition to opening up the
then allow it to dry before examination. The Duron material slightly in order to clarify the structure, the
may be sprayed on, but this has the disadvantage of impregnation also helps to support the fibre and preserve
giving droplets on the specimen. structure during sectioning.
It should also be noted that it is often possible to Another swelling and staining technique is described
examine specimens as received without any antistatic by Sotton et al. 13-15. Fibres are first exposed to hydrogen
treatment, if the viewing conditions are carefully chosen. sulphide under pressure and then reacted with silver
In general, the choice of viewing conditions involves a nitrate. Some examples are shown in Figure 9.
compromise and, in any except the easy specimens,
effort spent in securing the best compromise in relation Dark-field (diffraction contrast)
to the type of specimen and the needs of the investigation Where a specimen contains crystalline regions, contrast
will do much to improve the results. The parameters can be generated by dark-field viewing. By selecting one
available for variation are accelerating voltage, beam part of the diffraction pattern, and using it to form the
current, lens currents, aperture sizes, viewing distance, image, crystallites with a particular orientation show up
astigmatism correction, and exposure time: these interact as bright patches. Ingram10,11 has used this method to
together to influence resolution, contrast, depth of focus, show up continuity of orientation over lengths of about
penetration and spread in specimen, charging troubles, 40 nm in fibrils in cellulose fibres; but he points out that
specimen damage, and specimen movement or vibration it is difficult to get good results because cellulose is very
error. These problems and, in particular, the advantage susceptible to electron damage, and so it is necessary to
of using relatively low voltages for fibre examination are use a low beam intensity, which with weak diffraction
discussed by Hearle et al.8. gives a very weak signal.
The plate method is an easy method for examining Earlier, Peterlin et al. 16 applied the technique more
fibre cross-sections. The individual fibres, or the yarn, successfully on laboratory-prepared specimens of poly-
are surrounded with a bundle of packing yarn, and then ethylene, but it is a technique which might be explored
pulled through a hole in the stub with a wire or strong more in studying synthetic fibre structure.
yarn. The surface is then cut flush and coated. It is
necessary to ensure that the yarns are tightly packed Disintegration
before cutting. Another way of studying fine structure is to break up
Comments on disintegration, peeling and sectioning of the fibre. The classical methods are well-known and
fibres have already been made in connection with direct have already been mentioned. A comparatively new
electron microscopy. method, utilizing the X-press equipment of Biotec,
Some examples selected from our studies at UMIST involves forcing a frozen mixture of water and fibres
using these methods are shown in Figure 8. through an orifice under high pressure. The principles
The X-ray emission mode is being used for identifica- were described by Edebo 17. At -25°C and 2x 105kg/
tion of location of finishes, soil particles etc. Cathodo- mm 2, ice undergoes a crystal lattice transition. At the

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Electron microscopy of textiles: J. W, S. Hearle and S, C. Simmens

Figure8 Examples of scanning electron microscope studies of textiles. (a) Cross-sectional shape of cellulose acetate fibres by the plate
method; (b) wool fibre; (c) internal surface of nylon-6 filament revealed by peeling; (d) bonded-fibre fabric; (e) conventional (ring-frame)
cotton yarns; (f) comparative study of break-spun yarn; (g) cotton-polyester blend fabric, showing general structure and singed fibre
ends; (h) used cotton-nylon sheets showing fibre damage. [From work of B. Lomas, B. H. Bhutta and K. L. Ghandi (UMIST)]

278 POLYMER, 1973, Vol 14, June
Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens

Figure9 Use of staining methods by SottonZ3-zS--treatment with HzS followed by AgNO3 to show structural differences. (a), (b) stained
acrylic fibres; (c), (d) surface region of polyester fibres. (Pictures by courtesy of M. Sotton, Institut Textile de France)

moment of the transition there is a degree of mobility High-voltage electron microscopy
which allows some material to pass through a small If the fibre will survive examination, high-voltage
orifice. The high pressures serve to disintegrate the electron microscopy can be used on complete fibres.
fibres. Some examples are shown in Figure 10. Sharp and Burnay 18 have used the method to examine
There are interesting differences between fibres. Nylon carbon, metal and ceramic fibres. Figure 11 shows two
is barely affected by 10 passes, but du Pont's fibre B views of the same fractured carbon fibres, seen in a
splits readily into fibrils. The illustrations demonstrate s.e.m, and at 1 MV in the high-voltage transmission
how, in this application, the s.e.m, runs out of useful microscope. The internal void shown in the high voltage
magnification between 2000x and 20 000 x , but the picture can be related to external features visible with the
direct electron microscope can go on to higher magni- s.e.m.
fications. There are also differences in appearance in Only thin specimens of the comparatively low-melting
the two microscopes. Viscose rayon splits into short polymers used for textile fibres can be examined in the
pieces. Untreated cotton fibrillates, with some difficulty, high-voltage microscope. Thick specimens, such as whole
but resin crosslinked cotton breaks into short pieces. fibres, melt quickly owing to the energy absorption. It
Acrylic fibres (not illustrated) vary in their ease of is possible that scanning high-voltage microscopy might
fibrillation. solve this problem.

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Figure 10 Use of X-press method on fibres. (a) Nylon, after 10 passes, showing little change apart from distortion due to buckling (s.e.m.);
(b) fibre B, after 10 passes (s.e.m.); (c) fibre B, after 10 passes (s.e.m. higher magnification); (d) fibre B, after 10 passes (direct electron
microscope); (e) fibre B, after 10 passes (direct electron microscope, higher magnification); (f) viscose rayon, after 10 passes; (g) cotton,
after 2 passes; (h) resin crosslinked cotton after 2 passes. [Pictures by B. Lomas and J. T. Sparrow (UMIST) and S.C.S.)]

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Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens

Figure 11 (a) High-voltage transmission electron microscope view of a fractured carbon fibre; (b) s.e.m, view of fibre. (Pictures by courtesy
of d. V. Sharp, AERE, Harwell)

S.e.m. flming features which are invariant in a variety of ways of
The use of TV-scanning to show up dynamic experi- examining or preparing the specimen are more likely to
ments on fibres and textiles is a very useful technique. be real and not artifacts. There are many possible vari-
At U M I S T Hearle et al. lo have preferred to use lapsed- ations on this theme: through-focusing as shown in the
time cinephotography in order to show up the sequence Leeds exhibit 21, change of viewing conditions, use of
of events in, for example, the extension and failure of different knives in sectioning, use of different stains or
bonded-fibre fabrics, the deformation of yarns and swelling agents, the combination of studies with quite
knitted fabrics, and the fracture mechanisms of cotton different modes of preparation and examination etc.
fibres.
TWO CURRENT TOPICS
Reliability of information
There are many applications of electron microscopy Fine structure of fibres
to fibres where there is little difficulty in interpreting the In both natural and synthetic fibres there remain
results, but there are also many interesting problems interesting problems of fine structure concerning which
where the method may be pushed to a limit and where electron microscopy has already provided some clues,
doubts arise. A due degree of scepticism is a virtue. and should yield more, but which remain unsolved.
The errors due to specimen damage during preparation Rather curiously, the structural situation is qualitatively,
or viewing, to charging, and to similar causes are fairly if not quantitatively, clearer for the regenerated cellulose
well appreciated, if not always understood. But, near fibres. The two important groups of natural fibres--
the limit of resolution, it is important to consider the cotton and other plant fibres, wool and other hair fibres--
nature of image formation. Lipson and Lipson 2° have have very different structure but in both the wealth of
recently pointed out the difficulties which arise from gross structural features are well-established and there
the strong interaction of electrons with matter, and is clearly a fibrillar fine structure at a level of the order
which may upset the usual theory of image formation of 10nm; what is uncertain is whether there are appreci-
as a simple pair of Fourier transforms. They state that ably finer fibrillar units. In the melt-spun synthetics
the limit of resolution will be about 4 (;~t)1/2, where A (acrylic fibres are rather different) the structure is gener-
is the electron wavelength and t is the specimen thickness. ally more uniform over the whole fibre, except possibly
For specimens of thickness 1000/~, this indicates a for a skin; what is uncertain is whether the fine structure
resolution of about 30,~. Images, such as those of is a comparatively uniform system of intermediate order
lattice planes in carbon fibres, with apparently well- (paracrystalline, a highly defective crystal, or amorphous
resolved smaller spacings are really Young's fringes, with correlation) or whether it contains recognizable
and not actual images of the object. This is pointed out crystallites and, if so, whether these are fibrillar, micellar
in work at Leeds University 21. or even lamellar. The varying views of synthetic fibre
In order to overcome the possibilities of misinterpreta- structure are not necessarily exclusive: the structure may
tion in difficult cases, more use might be made of careful differ according to the history of fibre formation and
searching for invariance under transformation. Those subsequent treatment. In the family of rayon fibres, we

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Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens

/
II
Figure 12 Fibril of cotton (65 000×) (S.C.S.). Short sections, located on the line diagram, are shown to allow adequate magnification in
the print
can interpret the difference between fibres which are electron microscope pictures is not easy or unambiguous,
formed by direct crystallization (precipitation) from and Preston 2s argues strongly that the basic fibrillar
solution, followed by stretching, and those which are units are thicker. Evidence from other sources (X-ray
formed by crystallization in the oriented solid state as diffraction, chemistry, biosynthesis) is inconclusive or
being a difference between a micellar and a fibrillar conflicting.
texture. In wool, fibrillar disintegration does not easily occur,
In natural cellulose fibres, there is clearly a coarse but the staining of sections shows micro fibrils about
fibrillar structure, and this breaks down into separate 70A in diameter spaced 100A apart in a matrix (Figure
fibrils. The problem of the identity of the ultimate micro- 14). A wealth of circumstantial evidence identifies the
fibril is well illustrated by Figures 7 and 12, which show microfibrils with helical crystalline material made of
cotton mechanically disintegrated in a blendor. In low-sulphur protein and the matrix with amorphous
Figure 12, there is an enormous length of a fibril, about material of high-sulphur (cystine crosslinked) protein.
7/~m, with lateral dimensions of about 120A; but at There is believed to be a continuity between the helical
the end, it splits into finer fibrils. The question is whether segments of chains in the microfibril and their tails in
these represent a smaller basic unit (a protofibril), or the matrix. In the stained cross-sections, the eye of faith,
whether they are merely the result of cleavage between looking with some reason for double or triple helices,
the molecules in the coarser fibrillar crystallite. Examina- can see indications of a protofibrillar internal structure
tion of the residue left on evaporation of the liquor of the microfibrils; but interpretation of the electron
shows globular particles which may well be single micrographs at this level is difficult, though Fraser et
molecules resulting from the ultimate splitting of the aL 24 have shown that it can be helped by optical filtering.
crystals. Thus there is doubt about evidence from disinte- More convincing evidence came with the apparent
gration studies, even if one can accept the measurements isolation of protofibrils by disintegration of wool. How-
of the size of the protofibrils, near the limit of resolution. ever, Millward ~5 and Fraser et aL ~6 have shown that the
Fibrils can be shown up in thin sections, or disintegrated 'protofibrils' can arise from contamination of the
lamellar fragments, by developing contrast by the staining specimen with cellulose--providing, incidentally, in their
methods mentioned earlier, as shown in Figure 13. studies of disintegrated Kleenex tissue some of the best
ingraml0, zl states that this suggests that the secondary pictures of finer cellulose fibrils. Dobb and Sikorski 27, 28
walls in cotton are lamellae consisting of partly coalesced do not accept that the observed protofibrils always arise
fibrils of about 50A in lateral width. Manley 22 has in this way. They show by selected area electron diffraction
proposed very specific crystallographic modes of fibre that fragments from a disintegrated Merino wool fibre
formation, and finds support in his electron microscope were indeed keratin; however, these were relatively
studies. However, the detailed interpretation of the large sheets not isolated protofibrils and, as in other

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structure. Rather coarse fibrils are seen in some peeled
fibres, but this may reflect the influence of fluctuations
within the coagulating stream during fibre formation
or in the fibre during drawing, or it may be an artifact
of peeling mechanics. The staining methods of Van Veld
et al. 2a do apparently show a fine fibrillar texture, not
very clearly resolved, with nodes along the fibre. Hearle
and Greer 30 have suggested that this may be the result
of the aggregation of micelles in pseudo-fibrils.
More comprehensive studies, using many techniques
including electron microscopy, on a set of well-charac-
terized samples are needed to establish the nature of the
fine structure of these fibres. It is likely that if the same
effort was put into the electron microscope study of
synthetic fibres as has been put into cotton and wool,
useful results would ensue. For the ignorance about
synthetic fibres is related to structure at the level of
10 to 20nm, in contrast to the finer level where the
uncertainties now rest with the natural fibres.
At first sight, the disintegration of fibre B shown in
Figure 10, might seem to be convincing evidence of a
fibrillar fine structure. But there does not appear to be
any limiting preferred size for the fibrillar units, and it
is more likely that what is observed is merely a splitting
between molecules in a very well-oriented fibre. The
splitting would continue on down to a molecular level,
just as a crystal of mica goes on splitting, and so would
Figure 13 Stained section of ramie (122500x). (Picture by only be evidence that the material is a highly ordered
courtesy of P. Ingram, ResearchTriangle Institute, North Carolina)
linear polymer.
In order to check whether an observed fibrillar struc-
ture is evidence for a real fibrillar unit in the fibre before
disintegration (or other specimen preparation), it is
necessary to check, either by casual observation or more
explicitly, whether there is a statistical predominance of
fibrils of a particular size. If there is a sharply peaked
distribution then this is evidence for a basic fibrillar
unit; if there is a continuous broad distribution of sizes
it is evidence against.

Fibre fractography
The advent of scanning electron microscopy has
opened up the subject of fibre fractography, and has
been the most important aspect of our s.e.m, work at
UMIST. Because it shows the whole specimen in focus
(as compared with the very limited depth of focus in an
optical microscope) the general features of fibre fracture
are clearly visible in s.e.m, views and, in addition, much
fine detail can be examined at higher magnification.
The work is important for several reasons: (a) for its
general scientific interest; (b) for the insight into mecha-
Figure 14 Stainedsection of wool. [Reproducedfrom d. Textile nisms of failure in fibres, and thus as a guide to the
Inst. (1969,60, 498) by permission of the Textile Institute]
possibility of improvement of fibre properties by the
fibre producer; (c) for the insight into the causes of
such specimens, the evidence that they were composed failure in use and processing and thus as a guide to
of 2 n m filaments does not seem conclusive. At the improvement in processing methods or into construction
moment, it is difficult to avoid taking the view that while of yarns, fabrics and garments; (d) as a means of diagnosis
protofibrils may exist in wool, there is no convincing of causes by failure.
evidence for their existence. The results can be briefly summarized by a classifica-
The main evidence against a fibrillar fine structure in tion of the forms of fracture which have been observed.
polyamide and polyester fibres is the difficulty of pro- There are, however, many variants and combinations of
ducing fibrils by fibre disintegration or fracture--in the basic forms, and a full account of the work is, or
comparison, for example, with the ease with which will be, contained in other papers, including a continuing
fibrillation occurs in cotton or wet-spun acrylic fibres. Atlas of pictures al.
This would suggest that the structure is a partially The fibre fractures, so far observed, can be divided
ordered network of shorter elements or a micellar into the following classes.

POLYMER, 1973, Vol 14, June 283
Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens
Elastic crack growth fractures. Glass fibres show the
classical brittle fracture from a Griffith's crack; similar
fractures, though with large deformation, may occur in
the tensile failure of elastomeric fibres. In these instances,
the crack becomes less stable as it grows.

Ductile crack growth fractures. In nylon and other
synthetics, as described by Hearle and Cross 32, the crack
growth is accompanied by drawing of the remainder of
the cross-section and so the crack opens as a V-notch
before the final catastrophic failure occurs (Figure 15).
In this case, the crack requires a greater load for propaga-
tion the deeper it gets; this is a situation in which more
detailed analysis of fracture mechanics is required. On
rare occasions fracture of this type is initiated at an
interior flaw.

Fractures with axial splitting. In the tensile fracture of
cotton, described by Hearle and Sparrow aa, and in the
torsional fracture of some acrylic fibres, the dominant
feature is a splitting of the structure along its length as
shown in Figure 16. This is associated with the marked
fibrillar nature of these fibres.

Axial splitting due to fatigue. Hearle and Bunsella4
have shown that tensile fatigue can cause cracks to run
along the fibre parallel to the tensile stress axis, giving
breaks with long tails as shown in Figure 17. In order to
promote this fatigue failure in nylon it is necessary that
the load should fall to zero in each cycle. With a peak
load much less than the normal breaking load, failure
occurs in 10 5 to 10 6 cycles, owing to an initial surface
crack turning and running along the fibre, getting gradu-
ally deeper. In polyester and acrylic fibres long internal
cracks develop.

Fracture perpendicular to the fibre axis. Rayon, acrylic
fibres, wool, and crosslinked cotton show breaks which
run across the fibre with no clear crack morphology and
moderate roughness. An example is shown in Figure 18.
Sometimes, there is a marked discontinuity along the

Figure 16 Cotton tensile fracture. [Picture by J. T. Sparrow
Figure 15 Nylontensile fracture. [Picture by B. Lomas (UMIST)] (UMIST)]

284 POLYMER, 1973, Vol 14, June
Electron microscopy of textiles: J. W. S. Hearle and S. C. Simmens
or have their ends melted or chemically attacked. It
also includes fibres broken to make staple fibres and
fibres which have failed in use.
As the work proceeds, other forms will, no doubt, be
recognized.

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3 Dlugosz, J. Proc. 1st Eur. Reg. Conf. Electron Microsc., Stockholm
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4 Ramanthan, N., Sikorski, J. and Woods, H. J. Proc. Int. Conj.
Electron Microsc., London 1954, p. 482
5 Scott, R. G, A S T M Spec. Tech. Publ. No. 257 1959, p 121
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7 Chippendale, P. J. Text. Inst. 1960, 5 (11), T392
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30 Hearle, J. W. S. and Greer, R. J. Text. bzst. 1970, 61,243
Figure 18 Acrylic fibre tensile fracture. [Picture by B. Lomas 31 'An Atlas of Fibre Fracture', (continuing series) Text. Manuf.
(UMIST)] 1972 (.January), No. 1
32 Hearle, J. W. S. and Cross, P. M. J. Mater. Sci. 1970, 5, 507
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in scale, the fracture of fibre-reinforced composites and
is probably due to the separate rupture of fibrils within
General references
the fibre.
J. A. Chapman in 'Physical Methods of Investigating Textiles',
Failure from kink-bands. Fibres in compression, for (Eds J. W. S. Hearle and R. Meredith), Interscience, New York,
example on the inside of a bend, develop oblique bands 1959, Ch 3
'Fibre Structure', (Eds J. W. S. Hearle and R. H. Peters), Butter-
visible in polarized light. Under repeated flexing, failure
worths, London, 1963
occurs along these bands. This is an area of current study. J. W. S. Hearle and R. Greer, Text. Progr. 1970, 2, (4)
'The Use of the Scanning Electron Microscope', (Eds J. W. S.
Other breaks orfibre ends. This is a miscellaneous group Hearle, J. T. Sparrow, and P. M. Cross), Pergamon Press, Oxford,
not separately classified. It includes fibres which are cut, 1972

POLYMER, 1973, Vol 14, June 285