SELF-HEALING OF COMPOSITE STRUCTURES IN A

SPACE ENVIRONMENT
R S Trask1, I P Bond1 and C O A Semprimoschnig2
1
Department of Aerospace Engineering, University of Bristol,
Queen's Building, University Walk, Bristol. BS8 1TR. U.K, R.S.Trask@Bristol.ac.uk
2
European Space Agency, ESTEC, Materials Physics & Chemistry Section PO BOX 299, Keplerlaan 1,
NL - 2200 AG Noordwijk, The Netherlands. Christopher.Semprimoschnig@esa.int

ABSTRACT to-hole size are often observed for carbon/epoxy

laminates) [3].
The use of functional repair components stored inside
hollow reinforcing fibres is being considered as a self-
Space composite laminates can also suffer from
repair system for future composite structures. This
internal matrix microcracking. This type of damage can
paper considers the problem of introducing a liquid
occur within the lifetime of the composite structure due
healing resin, contained within hollow glass storage
to its exposure to the repeated thermal cycling within
vessels, within a space environment. The problem of
the space environment. The magnitude of the
resin outgassing of a commercially available 2-part
microcracks will be dependent upon certain laminate
epoxy resin system and the thermal cycling of the glass
and environmental properties (i.e. mission orbit,
storage vessels, and their sealing caps, are discussed.
thermal properties, fibre and resin properties, number
The mechanical property assessment of the baseline
of cycles, stacking sequence, temperature differential,
hollow fibre laminate, the damaged hollow fibre
bond strength, stress/strain at micro/macro levels and
laminate and the healed hollow fibre laminate is
matrix morphology). Any form of self-healing system
discussed revealed that a self-healed laminate had a
contained within a space composite laminate must be
residual strength of 87% compared to an undamaged
able to repair damage resulting from collisions with
baseline laminate and 100% compared to an
micrometeoroids and orbital debris or damage arising
undamaged self-healing laminate. This study provides
from thermal cycling.
clear evidence that a FRP laminate containing hollow
fibre layers can successfully self-heal.
2. SELF-HEALING REPAIR OF SPACE
1. INTRODUCTION
COMPOSITE STRUCTURES
Terrestrial composite structures can be damaged in
The use of functional healing components stored inside
many ways, e.g. unexpected mechanical overload,
composite materials to restore physical properties after
fatigue loading at stress concentrations, heat/chemical
damage has been advocated since the 1990s [4].
attack or impact damage arising from collisions
Incorporation of hollow glass fibres within a structural
between moving objects. Foreign object impact to
composite laminate offers the advantage of being able
single skin laminates can result in a drastic reduction in
to store additional functional components for
composite strength, elastic moduli, and structural
composite self-repair systems [5]. To extend the
durability and damage tolerance characteristics.
existing terrestrial self-healing concept for composite
structures operating in space, certain aspects of the
Composite structures operating in the space
environment, the nature of the damage threat, the
environment are vulnerable to impact damage resulting
location of the hollow filaments, and the choice of
from collisions with micrometeoroids and orbital
repair resin have to be considered before a technical
debris. The relative velocity of man-made debris
solution can be derived.
ranges from zero, for objects in the same orbit, to
approximately 11 km/s for objects in retrograde orbits
In this research programme the self-healing is defined
[1]. In comparison, collisions with meteoroid particles
as autonomous, i.e. all the healing materials are
take place with an average velocity of 19km/s [2]. The
contained within the composite and no external repair
damage to the brittle composite structures consists of
is required to initiate the repair. Alternative repair
penetration holes with adjacent surface damage and
methods could be active autonomous healing which
some internal ply delamination. The internal damage
requires the replenishment of the healing medium or
may be anisotropic, following the structure of the
non-autonomous self-healing which requires some
fibres. For complete penetrations the rear surface
external impetus to initiate the repair.
damage area (surface spallation) is frequently larger
than the entry hole (ratios of 5:1 for spallation damage-
In the self-healing approach adopted by Bristol
University, hollow glass fibres are used because they
offer the advantage of being able to store additional
functional components for composite self-repair
systems as well as acting as reinforcement. This
approach has been investigated by a number of workers
[6-10]. A typical hollow fibre self-healing approach
used within composite laminates could take the form of
fibres containing a one-part resin system, a two-part
resin and hardener system or a resin system with a
catalyst or hardener contained within the matrix
material. The approach at Bristol has been illustrated in
Figure 1. This figure shows (top left) the 30m hollow
fibres, UV dye emitting from a fracture plane in a
hollow fibre composite (bottom left) and the healing
sequence of 2-part epoxy resin with UV dye using time
lapse photography (right).
Fig. 1: Healing process using hollow fibres; Top left -
30m hollow fibres, Bottom Left - UV dye emitting
from a fracture plane in a hollow fibre composite; and,
Right - the healing sequence of 2-part epoxy resin with
UV dye using time lapse photography (right).
The exact nature of the self-healing method will
depend upon (1) the nature and location of the damage,
(2) the potential self-healing repair resins, and (3) the
influence of the operational environment. The self-
healing fibres could be introduced within the composite
laminate as additional plies at each interface, at critical
interfaces or as individual filaments spaced at
predetermined distances within each ply. In this
research project, the self-healing filaments were
introduced at four critical ply interfaces were identified
within the same project and reported previously in [11].
In this research project an epoxy resin system (Cytecs
Cycom 823) was selected as the healing resin. This
system was chosen for a number of reasons. These
include the need to match the composite baseline
laminate (epoxy 913 with E-glass reinforcement), the
two part nature of the system permitting its inclusion in
separate storage vessels, the viscosity drops to a
minimum within the operating temperature profile, and
the mixed system reaches gelation within 30 minutes.
Furthermore, it was observed experimentally that the
individual elements of the 2-part system were
sufficiently robust to survive the composite laminate
curing processing route (120C for 1 hour) whilst
housed at their respective interfaces within the fibre
stack of the composite laminate. Although a carbon
fibre or glass fibre composite laminate could have been
selected as the baseline material it was decided to
select a glass fibre laminate since it permits better
visualisation of the damage when viewed with
transmission light. To enhance the visualisation UV
dye can also be used.
Finally a comment concerning the damage introduction
method should be made. Although the damage event
within the space environment is likely to be initiated by
either a high velocity impact or thermal cracking it was
decided that these two approaches were beyond the
scope of this project. Instead, a static three point bend
test fixture was used to initiate the damage (shear
cracks and delaminations) within the composite
laminates. Although the damage would not be
representative of the damage observed in the space
environment it would permit a repeatable evaluation of
the self-healing approach.
3. VERIFICATION OF THE SELF-HEALING
APPROACH IN A SPACE ENVIRONMENT
The space environment significantly influences the
selection and performance of the different candidate
resin systems. In the high vacuum of space, composite
materials desorb moisture, which can lead to large
dimensional changes in the structure. Alternatively, the
high vacuum environment of space can initiate the
mass loss of polymeric materials due to outgassing of
low molecular weight components. All composite
materials are assessed to determine the level of
outgassing with the aim of minimising this risk to
avoid the threat of contamination to mission critical
spacecraft components (e.g. optics). Clearly, a liquid
resin system exposed to high vacuum is likely to have a
high outgassing rate. However, in the case of the
current self-healing approach, the only time the liquid
resin and hardener will come into contact with the high
vacuum is when the structure has been damaged.
Furthermore, when the resin comes into contact with
the hardener the curing process will be initiated and
therefore the rate of outgassing should decrease as the
liquid transforms to a solid. To evaluate what takes
place under these circumstances an outgassing
experiment investigating the resin, hardener and the
mixed resin and hardener was devised. (a)

4. OUTGASSING TEST EVALUATION

The standard screening test method employed by ESA (b)
to determine the outgassing performance of candidate
space materials is given in document ECSS-Q-70-02A
[12]. This document describes a thermal vacuum test to
determine the outgassing properties of solid materials
proposed for use in the fabrication of spacecraft and
associated equipment. The test defines the outgassing
properties of materials at 125C under 10-3 Pa for 24
hours. This is determined by measuring the sample
before and after the test to ascertain the recovered mass
loss (RML) (i.e. total mass loss of the specimen
without the absorbed water), and the collected volatile
condensable material (CVCM) collected on a (c)
condenser plate in close proximity to the sample. The
collector plate was kept at a constant 25C during the
Fig. 2: Outgassing test set-up: (a) Al-foil crucible
experiment.
containing the mixed resin system; (b) Knudsen cell
with heater and thermocouples housing the Al-foil
The outgassing test method (as specified in ECSS-Q-
crucible; (c) Vacuum chamber housing Knudsen cell
70-02A) tends to be conducted on solid materials with
connected to mass spectrometer.
very low outgassing rates. However, since a two-part
liquid system (with potentially high outgassing rate)
Prior to the commencement of the outgassing
was going to be assessed it was decided to undertake
experiment the Cycom 823 liquid resin and hardener
some measures to avoid excessive contamination of the
where mixed at the recommended 4:1 ratio. At room
highly sensitive test equipment. A sample of material
temperature the mixed sample has a viscosity of 250cP
was placed in a bespoke, single Knudsen cell, which
and will not reach full cure for 6 days. A measured
was placed in a small vacuum system equipped with a
amount of mixed resin is then poured into a small
cold trap and evacuated by a turbo-molecular pump. In
Aluminium-foil crucible (see Fig. 2a). The crucible is
addition to capturing the mass loss, a mass
then placed in a small Knudsen cell, provided with a
spectrometer was used to investigate the nature of the
heater and two thermocouples (see Fig. 2b).
outgassing products as the temperature of the Knudsen
cell was slowly increased to 125C. The experimental
The Knudsen cell is contained within a small, vacuum
arrangement is indicated in Fig. 2.
chamber, which was evacuated by a two-stage, rotary
vane, mechanical pump. This provided a typical
pressure throughout the test of between 2x10-2 and
6x10-3 millibar. From the low-vacuum stream, a sample
of the gas was removed via a needle valve into a high-
vacuum system, pumped by a turbo-molecular pump.
The high-vacuum system operated at typically not
more than 2x10-5 throughout the testing. This system
was equipped with a high-vacuum gauge and a mass
spectrometer which was used to monitor the volatile
components from the samples throughout the test. Four
tests were undertaken to understand how the liquid
resin and hardener were affected by temperature and
vacuum. The first two tests considered the liquid resin
and hardener whilst the third and fourth tests
considered two different heating rates (at 3.33C/min
and 1.67C/min) for a 4:1 resin-to-hardener mix ratio.
The test results for the fast ramp rate have given below.
 Temperature [C]
25 26 35 41 48 56 64 70 76 92 100 106 113 119 125
Partial pressure 10^-7 to 10^-6

10
9
8
7
6
Torr

5
4
3
2
1
0
0 3 5 7 9 11 12 14 16 20 22 23 25 27 31
Time [minutes]

Hydrogen Methane H-carbons CO2 45

Fig. 3: Recorded partial pressures for Cycom 823 mixed resin system at fast ramp rate (RT to 125C in 30 minutes) for
specific elements and mass index numbers

The experimental data indicated in Fig. 3 is a measure Table 1: Mass loss measurements for Cycom 2-part
of the rate of outgassing of the different chemical epoxy liquid resin ramped to 125C within 60 minutes
elements as a function of temperature within the partial and held for 24 hours
pressure range of 10-7 to 10-6 Torr (a range chosen
specifically to capture the outgassing of the high mass Outgassing property description Mg
index elements). In general, the recorded spectra size Total specimen mass before test Wo 473.98
of the individual mass index number (MIN) in the fast Total specimen mass after test Wf 409.57
temperature ramp is higher than the corresponding Mass of material before test Wm 448.10
MIN in the slow ramp test, i.e. the accelerated rate has Final mass of collector plates after
induced rapid outgassing. The fast ramp rate results test Wg 61.24
indicated in Fig. 3 show a rapid increase in the Initial mass of collector plates
before test Wp 60.53
formation of hydrocarbon products from 76C to
113C before the rate of outgassing returns to the
Wo W f
baseline level once the material has attained 125C. TML % = 100 (1)
The reduction in the measured outgassing products is Wm
due to cure of the healing resin (typically 15 minutes
after attaining 95C according to manufacturers
data). Wg W p
CVCM % = (2)
Wm
In addition to the experiments to determine the
outgassing behaviour of a two-part epoxy RML
measurements were taken according to the test The TML of the liquid specimen over 24 hours was
guidelines in ECSS-Q-70-02A. In this standard, the 14.4% as calculated by Equation (1). The CVCM of the
general acceptance limits for outgassing materials (not two-part epoxy system over 24 hours was 0.16% as
manufactured for optical devices, or in their vicinity) calculated by Equation (2).
for RML is < 1% and for CVCM is < 0.1%. The mass
loss measurements for the Cycom 823 system are As expected, the outgassing performance of the liquid
detailed in Table 1. epoxy resin system falls outside the existing ESA
guidelines, i.e. guidelines generated for cured materials
and not for liquids. In the context of producing a self-
healing material, the Cycom 823 two-part resin system
was selected because it has a very low viscosity and The samples were inspected before and after the test
resin gelation occurs within 15 minutes at 90C. For a with the vacuum pump output being monitored using
standard commercially available epoxy resin this mass spectrometry to give an indication of any filament
system provides the best healing attributes within the rupture (i.e. tube fracture will release molecules that
operating environment. will be detected by mass spectrometry, providing an
indication of elapsed cycles before rupture).
It has to be stated that this test is the worst case for a
cracked hollow fibre. An undamaged and sealed fibre
shall be mostly impermeable to outgassing. As in a full End capped
composite the amount and mass of uncured resin in the hollow fibre
hollow fibre will be only a fraction of the total mass of Thermocouple
a composite the derived values have to be seen in a
perspective and therefore the obtained results are over-
estimating the outgassing of a full composite.
Furthermore, if, as the outgassing tests suggest, the rate
of cure can happen fast enough then the rate of
outgassing then the relative magnitude of the
outgassing products will be diminished even further.
To confirm the observation this phenomenon will need Liquid N2 Heater plate
further investigation. Cooling channel

A point to mention though is the question whether a

pressure build up within the hollow fibre could lead to
cracking or whether micro-cracking of the hollow
fibre/encapsulant could trigger any detrimental
outgassing reactions. To asses whether this is likely to
occur a series of thermal cycling tests were undertaken
to evaluate the thermal stability of the storage vessels
and two different end capping materials. The results of
these tests are discussed in the next section.

5. THERMAL CYCLING OF THE SELF-

HEALING STORAGE FILAMENTS
Determining the adverse effect of operational
temperature extremes upon the self-healing filaments is
a key requirement for any self-healing concept in a Fig 4. Thermal cycling set-up; (a) hollow fibre with
space environment. end cap seal; (b) Al storage chamber with 10 cavities
each housing a 100m diameter fibre by 100mm long;
To assess the self-healing concept in this environment
(c) thermal cycling chamber
a purpose built test fixture was manufactured to assess
the structural continuity of the seal at the end of the
In this experiment two different end-capping methods
hollow fibres (see fig 4.). The specimens (10 individual
(2-part Cycom 823 epoxy and 1-part high modulus
hollow fibres each with an external diameter of 100m
silicone sealant [Bostik 100HMA]) applied to 10
5m) were cycled between 100C for 100 cycles at
different filaments was undertaken. The test was
a heating rate of 10C per minute. The ten samples
arranged such that a number of filaments contained (1)
were sandwiched in individual grooves in an Al block
air, i.e. they were unfilled, (2) filled with Cycom 823
(see Fig 4b). Three thermocouples were pushed up
resin or (3) filled with Cycom 823 hardener. This
inside the Al block such that they were only 5mm away
approach investigated any effect on the sealing method
from the internal cavity. The Al block had two
by the healing material within the hollow fibre.
channels machined in the bottom face to permit two
copper cooling pipes using liquid Nitrogen to be
In the first experiment difficulty with locating the
secured to the specimen block. The final assembly was
100m diameter fibres within their 100mm long cavity
located upon a heater plate. This arrangement
was experienced. This resulted with the loss of 2
permitted the temperature profile to be controlled using
storage tubes due to fibre crushing. These two failures
a balance between the heater plate and the liquid
were recorded by the mass spectrometer. Apart from
Nitrogen and eliminated any thermal lag.
the crushing failures no other failure was recorded
during the experiment of either the epoxy or silicon end
caps. When viewed under the microscope the
continuity of the end caps for both sealing methods was
confirmed.
The only significant difference between the two
methods was their ease of application and the
consistency of forming the meniscus at the end of the
hollow tubes. The high viscosity of the silicone system
is maintained throughout the room temperature curing
process and hence results in a controlled cap.
Conversely, the 2-part epoxy requires an increase in
temperature to initiate the cure. However, before
gelation occurs the resin system attains its lowest
viscosity value (15cP) thus making the control of the
end cap difficult. An example of the two different
sealing methods is given in Fig 5. In addition to the
process control problems the outgassing performance
of the silicone is superior to the epoxy and hence was
selected for further evaluation.
(a) (b) (c)
Fig. 5: End capping methods on hollow glass storage
vessels; (a) 2-part epoxy correctly sealing over
exposed end, (b) 2-part epoxy not sealing the exposed
fibre end, (c) silicone correctly sealing over exposed
fibre end.
In the second test ten samples were sealed with silicone
and tested using the same procedure outlined above.
The mass spectrometry was used to monitor the
samples throughout the experiment and didnt record
any failures. This was confirmed by visual examination
after the experiment was concluded.
6. MECHANICAL PROPERTY ASSESSMENT
6.1 Self-healing laminate manufacture
The hollow glass fibre diameter was chosen to have an
external diameter of 60 m 3 m and an internal
diameter of ~40 m yielding a hollowness fraction (the
ratio of internal area to external area) of ~55%. Once
manufactured the individual fibres are then
consolidated within a 913 epoxy resin film, which was
selected to match the baseline laminate material. The
healing resin can then be drawn into the individual
lamina using a vacuum. Once the ends have been
sealed (in this research the fibres were sealed with
Bostik Bond Flex 100HMA high modulus silicone
sealant) the infused hollow fibre layers (which can be
considered as standard prepreg sheets) are then laid-up
according to the required stacking sequence and
processed according to the manufacturers guidelines.
Once fully cured the laminate was sectioned into
individual samples measuring 25mm wide by 100mm
long. After cutting, the edges of the samples are sealed
with a two-part rapid curing epoxy system (Araldite
Rapid) to prevent any healing resin loss through the
exposed ends of the hollow fibres.
6.2 Flexural strength determination
Four-point bend flexural strength testing according to
ASTM D627202 [13] was selected to characterise the
strength and stiffness of the baseline and self-healed
samples. A detailed investigation of this work has been
reported previously [11], but for clarity a brief
summary will be given below again. The four-point
loading configuration ensures a region of uniform
bending stress in the area of the damage between the
loading noses, rather than a peak stress under the nose
at the point of worst damage. A support span to depth
ratio of 32:1 with the loading noses positioned at one
third of the span was selected. The tests were
conducted using a loading rate of 5mm/min on a Roell
Amsler hydraulic test frame fitted with a 25kN load
cell. A Linear Potentiometric Displacement Transducer
(LPDT) was used to record mid-span deflection, which
was logged through a PC running Instron data
acquisition software.
In the case of the damaged samples a three point bend
test was used to initiate matrix shear cracks and
delamination damage with the composite laminate. In
the case of the laminate containing the self-healing
resin and hardener lamina this was permitted to heal by
heating to 100C (from ambient) in an air circulation
oven and held at this temperature for 2 hours. This
curing cycle was selected to match the typical
operational temperature profile of a composite
structure in space undertaking two low earth orbits
(LEO).
The flexural strength results for the five different
laminate configurations (baseline, baseline + damage,
self-heal baseline, self-heal baseline + damage, and
self-heal baseline damaged + healed) are given in
Table 1.
Table 1. Summary of flexural strength and percentage-
retained strength
Flexural
Specimen strength
Specimen description
ID
[MPa]
Baseline laminate
Group A {[0/+45/90/-45]2s} 668 13 100
no damage
Baseline laminate with self-
healing layers at critical
Group B interfaces {45/90} 559 12 84
no damage
Damaged (2500N indentation)
Group C 479 32
baseline laminate
Damaged baseline laminate with
Group D self-healing layers, 494 7
no repair
Damaged baseline laminate with
Group E self-healing layers, with 2 hours 578 28
self-healing at 100C
The experimental results shown in Table 1 illustrate the
ultimate flexural strength and the percentage-retained
strength for the different sample configurations. The
results indicated that the inclusion of hollow fibres
gives in an initial strength reduction of 16%. It was
found that the baseline laminate (Group A) and the
laminate containing the hollow fibre layers (but no
healing) had comparable low energy impact damage
tolerance both in terms of damage size and residual
failure strength (typically 72-74%). After healing of the
damage site was undertaken it was found that a self-
healed laminate (Group E) had a residual strength of
87% compared to an undamaged baseline laminate
(Group A) and 100% compared to an undamaged self-
healing laminate (Group B).
7. CONCLUSIONS
This work has shown that a hollow-fibre self-healing
approach can be used for the repair of advanced
composite structures. In the course of this study it has
been shown that hollow glass fibres containing a two-
part healing resin can be manufactured and
incorporated within a standard autoclave processing
technique, thereby, indicating that this healing
approach could be readily applied to existing
composites manufacturing techniques. Through the
specific placement of four self-healing plies to match
the critical damage threat it has been shown that a
standard commercial available two-part epoxy resin
system (Cycom 823) can be used for the repair of
internal matrix cracking and delaminations through the
thickness of a 16 ply laminate.
The thermal outgassing of the 2-part Cycom 823 epoxy
resin system was observed to fall outside the existing
% ESA guidelines, i.e. guidelines generated for cured
materials and not for liquids. However, it has to be
retained
strength stated that this test is the worst case for a cracked
hollow fibre. An undamaged and sealed fibre shall be
mostly impermeable to outgassing since it will be
located within the heart of the composite laminate. A
final point to note concerns the selection of the healing
resin. At present a resin system specifically designed
for operation within the space environment does not
exist. For this research project, the Cycom 823 two-
part resin system was selected because it has a very
low viscosity and resin gelation occurs within 15
72
minutes at 90C. For a standard commercially available
epoxy resin this system provides the best healing
74 attributes of balancing low viscosity with relatively
quick gelation thereby permitting infusion of the
damage whilst minimising the extent of outgassing. A
87 resin system optimised for this environment would
clearly be more beneficial.
The thermal cycling tests illustrated the robustness of
the hollow fibre and the two different end capping
materials for surviving the LEO thermal environment.
A series of mechanical tests were undertaken to
evaluate the influence on the flexural strength of
incorporating hollow fibre plies into a baseline
laminate. The results indicated that the inclusion of
hollow fibres gives in an initial strength reduction of
16%. It has been shown that the damage site was
undertaken it was found that a self-healed laminate had
a residual strength of 87% compared to an undamaged
baseline laminate and 100% compared to an
undamaged self-healing laminate. This result would,
therefore, suggest that biomimetic repair is now
possible for advanced composite structures.
8. ACKNOWLEDGMENTS
The authors wish to acknowledge the financial support
of the European Space Agency, ESTEC Contract No.:
18131/04/NL/PA, throughout the duration of this
project.
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