Acta Astronautica 170 (2020) 466–471

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Acta Astronautica
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Research paper

Outgassing effect in polymeric composites exposed to space environment T

thermal-vacuum conditions
R. Pastorea,∗, A. Delfinib, M. Albanoc, A. Vricellac, M. Marchettib, F. Santonib, F. Piergentilia
a
Sapienza University of Rome, Department of Mechanical and Aerospace Engineering (DIMA), Via Eudossiana 18, 00184, Rome, Italy
b
Sapienza University of Rome, Department of Astronautics, Electric and Energy Engineering (DIAEE), Via Salaria 851, 00138, Rome, Italy
c
Italian Space Agency (ASI), Via Del Politecnico Snc, 00133, Rome, Italy

A R T I C LE I N FO A B S T R A C T

Keywords: Polymeric composites are widely adopted for design and realization of spacecraft components and subsystems,
Outgassing due to their lightweight and thermo-mechanical properties. However, the use of such materials for aerospace
Polymeric composites operations should be carefully conceived, since the detrimental effects they may experience within the severe
Space environment simulation space environment. A typical issue to be considered is represented by the outgassing phenomena a polymeric
Carbon fiber
composite suffers in ultra-high vacuum at elevated temperatures: in this harsh condition, a release of gaseous
Fiberglass
species from the material surface takes place, resulting in structural depletion and nearby components con-
Kevlar
tamination. The present work describes the results of outgassing tests carried out on three typologies of widely
used polymeric composites, such as epoxy matrix reinforced by carbon fiber, fiberglass and aramid fabric. The
experimental behavior of these materials is analyzed with the aid of infrared spectroscopy, in order to gain
knowledge about the chemical modifications that outgassing dynamics induce on the fiber-intercalated poly-
meric chains. The compliance to space assurance requirements – i.e., mass loss and condensed matter amounts
vs. standard outgassing rates thresholds – is discussed with regard to the different functionalities each material is
envisaged to accomplish, when applied onto space vehicle's exposed side. Further, in case of exceeding out-
gassing rate, a pre-treatment by thermal conditioning is proposed to improve the chemical stability of materials
in thermal-vacuum conditions, in order to explore the feasibility of their use for aerospace applications.

1. Introduction
Polymeric composite materials (PCMs) are extensively used in
aerospace industry, thanks to a bunch of desirable characteristics – such
as low density, high specific strength and stiffness, good insulation, low
thermal expansion coefficient, easy molding processing, etc. – which
make them ideal candidates for realizing high strength structural parts,
temperature control cladding, insulating paints, printed circuit boards,
optical fiber materials and so on, further reducing aerospace structures
assembly time and overall cost [1–7]. However, the extended operative
life that space vehicles, stations and satellites are expected to spend in
low earth orbit (LEO) regions demand for an excellent capability of
materials and components in retaining their performances for long
periods of time within the harsh space environment. For such reason,
the validation of PCMs for aerospace applications requires specific and
detailed ground-test activity by simulating the space operating condi-
tions, in order to assess how aging and degradation due to critical en-
vironmental factors (such as tough thermal cycling, high vacuum,
impact from space radiations, atomic oxygen, meteoroids and space
debris, etc.) would affect the PCMs thermo-mechanical, electrical and
optical properties [8–15].
In particular, considering the complex chemical reactions involved
in polymerization processing, it is well understood that dramatic
pressure lowering and temperature oscillations (as in space environ-
ment respect to standard T&P conditions) may seriously affect the PCMs
physical stability, cause the occurrence of outgassing phenomena.
Vacuum-induced outgassing is defined as the release of gaseous species
from a surface subjected to hard vacuum conditions, i.e. in so rarefied
atmosphere that the material's own vapor pressure is approached. The
ultra-high vacuum level of typical operative space environments (10−7
to 10−9 Pa in LEO regions, < 10−4 Pa inside satellites) is able to cause
the sublimation of exposed surface atoms, with subsequent drawbacks
of structural weakening and contamination. Such effect is mainly re-
levant in organic materials as PCMs, due to the presence of volatile
components as low-molecular weight residues, additives, plasticizers
and adsorbed gases, and can be greatly enhanced at the high

∗
Corresponding author.
E-mail address: roberto.pastore@uniroma1.it (R. Pastore).

https://doi.org/10.1016/j.actaastro.2020.02.019
Received 21 November 2019; Received in revised form 3 January 2020; Accepted 9 February 2020
Available online 13 February 2020
0094-5765/ © 2020 IAA. Published by Elsevier Ltd. All rights reserved.
R. Pastore, et al.
temperatures experienced during space thermal cycles (up and above
100 °C), because of the increasing of both materials vapor pressure and
chemical reactions rate [16–25].
Therefore, the evaluation of PCMs outgassing in high thermal-va-
cuum conditions is mandatory for ensuring the reliability of such ma-
terials for aerospace applications. In particular, the outgassing test
should provide information about the chemical nature of the expelled
gases, since these latter – by re-condensation – may lead to harmful
effects in aerospace missions where preserving nearby surfaces and
sensitive devices from contamination represents a crucial constraint.
Beyond the loss of mechanical performances by materials undergoing
outgassing, in fact, hazards like optical components and solar cells
obscuring, formation of local clouds affecting sensitive instrument
reading, pollution and corrosion of thermal control surfaces and passive
radiative cooling systems, etc., must be thoroughly reduced [26–30].
The identification of the products of condensation resulting from PCMs
outgassing under thermal-vacuum (moisture, dust, catalysts, mono-
mers, low-molecular weight fragments, etc.), as well as the analysis of
outgassing kinetics would be thus of vital aid for aerospace designers,
mostly as far as systems and subsystems around sensitive items (e.g.,
telescopes and optical sensors, detectors and cryogenic equipment) are
concerned.
In this work the thermal-vacuum characterization of three typolo-
gies of commonly used PCMs by means of certified outgassing equip-
ment is reported; the samples tested are representative of carbon fiber-,
fiberglass- and Kevlar-epoxy laminates manufactured by facile/low-cost
hand lay-up procedure. The experimental findings are discussed in
conjunction with the FT-IR spectral characteristics observed for the
tested PCMs, in order to establish indicatively the effective sources of
outgassing. The performances are also evaluated with regard to the
potential application planned for each kind of PCM in space structures
exposed to thermal-vacuum environment. Finally, the materials
showing unsatisfactory outgassing behavior – i.e., with mass loss and/
or condensable matter amount exceeding the standard thresholds – are
treated by thermal conditioning and re-tested by outgassing facility, in
order to assess a practical route to exploit commercially available PCMs
for aerospace applications.
2. Materials and methods
2.1. Polymeric composites manufacturing
The materials selected for outgassing testing are PCM laminates
made of a commercial epoxy matrix reinforced by three typologies of
common fibrous textile products – i.e., carbon fiber (CF), fiber-glass
(GF) and Kevlar fabric (KF). The matrix is the low-viscosity bi-compo-
nent epoxy Biresin® CR82 composite resin system (Sika Advanced
Resins), especially suited for hand lay-up process. Carbon fiber woven is
a biaxial woven roving 0°/90°, type HS CF k - dtex 450 g/m2 6 k 4/4
twill (Microtex Composites), fiberglass woven is a biaxial texture 0°/
90°, 600 g/m2 H.127 type 0–90 cm (3B E-Glass), Kevlar fabric is a 4/4
twill Batavia weave, type 49 Saatilar® style 103 loomstate - areal weight
of 635 g/m2 (DuPont™ Kevlar®). Large layered panel structures are
manufactured by integrating twelve plies of CF, GF and KF within the
polymeric matrix by hand lay-up method. The layers are resin-im-
pregnated by two-side brushing, and positioned on each other within a
mold by following the designed sequence; a pressure loading of about
7 bar is then applied over a square zone (25 × 25 cm2) of the as-
packaged multilayer, finally the curing process is carried on in oven
(50 °C for 16 h + 80 °C for 2 h). On average, fiber volume and weight
fraction within the range 0.80–0.85 and 0.75–0.80 are achieved, re-
spectively. In Fig. 1 the processing of the three materials for the panels
fabrication is pictured; small pieces are then retrieved from the panels
by water-jet cutting in order to provide samples of weight and dimen-
sion as required by outgassing test standard procedure.
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Acta Astronautica 170 (2020) 466–471
2.2. Outgassing test procedure
The outgassing test facility (OTF) available at Aerospace System
Laboratory (LSA – DIAEE/Sapienza Univ. of Rome) allows to perform
space materials tests in compliance with the outgassing ASTM and ECSS
standard references [31,32]. The test method covers a screening tech-
nique to determine the volatile content of materials when exposed to
vacuum environment at high temperature. The adopted OTF consists of
a vacuum chamber (Fig. 2) wherein the pressure may achieve values
down to 10−5 mbar by means of rotary/turbo-molecular pumping
system. Two metallic grids are allocated inside the chamber, facing
each other: a copper plate acting as sample-holders compartment is
connected to the electrical heating system used to raise the temperature
of the chamber up to 125 °C, while an opposing aluminum-chromium
coated plate is the collector box that can be maintained at 25 °C by oil-
cooling chiller equipment. The outgassing behavior of a specimen is
evaluated by measurements of weight, i.e. of the mass loss by vapor-
ization from the specimen's surface and of the amount of matter re-
condensed on the corresponding collector; the weights are measured by
means of a Mettler-Toledo XP26DR device (sensitivity 2 μg). Both the
OTF and the microbalance are located in ISO-7 certified clean room,
where all the test operations take place.
Before being inserted within OTF, the samples are kept for 24 h in
controlled conditions (23 °C, RH 50%, standard room pressure), in
order to unset mass variations due to previous handling/storage stages.
Instead, metallic sample-holders and collectors are subjected to a bake-
out cycle in ultra-high vacuum at 125 °C for 16 h, followed by further
conditioning in dry-vessel (RH 0%) at room temperature for 24 h, in
order to minimize unwanted weight losses during the test. After that,
the pre-test weight of all the objects is registered; then, the holders
(each containing a sample of weight in the range 100–300 mg) are fixed
in the hot grid hollows, while the collectors are locked to corresponding
slots on the cold plate. The chamber of the adopted OTF can accom-
modate twelve specimens for simultaneous testing, each specimen/
collector pair being isolated from the others by a compartmented se-
parator to prevent cross contamination; usually, two materials are
analyzed in a single test by inserting five samples for each typology
within OTF chamber, the two remaining spots on the plates being filled
with empty holders and cleaned collectors as blank reference. Hence,
the vacuum chamber is sealed and evacuated to a pressure around
10−5 mbar; at the same time, the specimen compartment temperature
is raised up to 125 °C (such hot temperature is selected to be about tens
degrees above any typical space operating temperature, in order to
provide accelerated aging effects), while the collector box is maintained
at 25 °C. Such condition is expected to cause vapor from the heated
samples to stream from the holes of their compartment toward the
cooled collectors, where a portion of the released gaseous species may
condense onto. The length of a standard outgassing test is 24 h; at the
end, the chamber is cooled and re-pressurized with dry nitrogen gas,
and then opened to collect sample-holders and collectors. These latter
are extracted from OTF by sterilized tweezers and promptly weighed:
comparing to the weights measured before the test, the ‘total mass loss’
(TML) and ‘collected volatile condensable materials’ (CVCM) are cal-
culated and expressed as percentages of the initial specimen mass (see
parameters definition in Table 1). Two more parameters may be eval-
uated after a further conditioning step, by storing the samples for
24 h at 23 °C and RH 50% to allow water vapor re-hydration, and fi-
nally weighting the samples again: the as called ‘regained mass loss’
(RML) represents the percentage of effective mass loss by outgassing
taking into account the weight recovery due to moisture sorption, while
the ‘water vapor regained’ (WVR = TML – RML) is the relative amount
of vapor re-absorbed by the sample. The criteria used for materials
acceptance is determined by the end-user and based upon specific
component and system requirements in terms of outgassing parameter
thresholds. Conventionally, TML of 1.00% and CVCM of 0.10% are
indicated as screening levels for rejection of spacecraft materials;
R. Pastore, et al. Acta Astronautica 170 (2020) 466–471

Fig. 1. Images of PCMs in-house manufacturing by hand lay-up method: a) final carbon fiber composite multilayered tile, b) fiberglass woven impregnation, c) Kevlar
ply brushing.

Fig. 2. Outgassing facility inside ISO-7 certified clean room @ LSA-DIAEE: a) open configuration (specimens fixing and removing), b) closed configuration (running
test), c) particular of the inner hot and cold plates.

Table 1 nevertheless, the restriction may be less or even more stringent de-
Outgassing parameters of PCMs tested by OTF: MS0 (MC0) and MS1 (MC1) in- pending on the structures assembly/functionality as well as on the
dicate the weight of samples (collectors) before and after the test, respectively, mission itself peculiarity.
MS2 is the sample weight after moisture re-absorption.
TML [ % ] (MS0 CVCM [ % ] RML [ % ] (MS0 WVR [ % ]
– MS1)/MS0 (MC1 – MC0)/ – MS2)/MS0 (TML – RML) 3. Results and discussion
MS0
The outgassing parameters of the PCMs tested in LSA-OTF were
CF – PCM 1.07 ± 0.11 0.07 ± 0.01 0.66 ± 0.09 0.41 ± 0.13
retrieved by sample/collector weight measurements, as summarized in
GF – PCM 2.46 ± 0.18 0.21 ± 0.05 1.76 ± 0.16 0.70 ± 0.21
KF – PCM 6.58 ± 0.32 0.71 ± 0.11 4.93 ± 0.27 1.65 ± 0.34 Table 1; the reported values are obtained by averaging on the results of
GFa – PCM 1.35 ± 0.15 0.13 ± 0.05 0.76 ± 0.09 0.59 ± 0.11 five specimens for each material, the uncertainties being taken as the
KFa – PCM 4.09 ± 0.23 0.52 ± 0.17 2.38 ± 0.30 1.71 ± 0.32 higher between statistical deviation and blank test result (this latter
representing the OTF actual sensitivity associated to a specific running
a
After fiber thermal pre-conditioning.
test).
Comparing to literature, in particular to what reported in official

468
R. Pastore, et al.
Fig. 3. FT-IR spectra of the several polymeric composite materials under test.
NASA database [33,34], the experimental findings confirm the fairly
good behavior of carbon fiber polymeric composites, which broadly
have acceptable outgassing rate; instead, fiberglass employment in
thermal-vacuum conditions should be deeply screened, whereas Kevlar-
reinforced materials present over-critical outgassing parameters. Thus,
basically, the proposed facile method sounds to be effective in produ-
cing CF-PCMs for application in space environment, while refined
technological routes would be required for the processing of GF- and
KF-based composites, if such materials are conceived to withstand
harsh thermal-vacuum conditions.
A FT-IR spectroscopy analysis was carried out to ascertain the kind
of chemical radicals present in the polymeric textiles used, in order to
assess the potential source of outgassed and eventual condensable
matter from the tested PCMs. A Varian 620-IR was used accordingly to
ASTM E1252 to obtain infrared spectra for a qualitative analysis be-
tween 4000 cm−1 and 400 cm−1, with resolution of 4 cm−1 and 128
scans averaged in the final spectrum. The FT-IR spectra retrieved by
analyzing the PCMs samples are reported in Fig. 3.
As main findings, the broadened peaks in the wave number region
3600-3300 cm−1 are associated to stretching vibration of hydroxyl
group (–OH), while the sharpen absorbance peaks around 1100-
1000 cm−1 are related to the bending of C–O bond. Such occurrence
would suggest the presence of water vapor and carbon oxides as main
constituent of outgassing content. Several absorption bands are re-
vealed at 2950 and 2850 cm−1, as characteristics of stretching oscil-
lation of C–H bonds. Absorbance around 1600 cm−1 are representative
of the stretching vibration of C]C, the C]O stretching vibration of
–NHCO and the N–H bending of –NH2, while at 1400 cm−1 O–H de-
formation and amide groups stretching vibration can be identified.
Finally, absorption bands characteristics of unreactive epoxy groups,
double bond of C]C and other aromatic bonds C–H can be detected in
the so called finger-print zone (below 1000 cm−1).
Comparing the relative intensities, it can be argued that the most
outgassing from CF- and FG-PCM is due to water vapor (O–H bonds
changing to H2O under temperature and vacuum), as well as to carbon
and nitrogen oxides; such gaseous species, in agreement to ECSS stan-
dard, are not considered as critical, their release (if not too exceeding)
not preventing the use of materials for aerospace applications. Based on
high TML and CVCM values found in OTF test, the more disordered
spectral response of KF-based material may be associated to other
gaseous releasing in addition to simple moisture and/or C-/N-ox
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Acta Astronautica 170 (2020) 466–471
species; mainly, unknown residual secretion (silicon oil or plasticizer
solvent treatments are often performed in Kevlar fabric production)
may be harmful, leading to dimensions instability, properties de-
gradation and surface contamination.
In spacecraft design, CF-PCMs are traditionally considered for pri-
mary and secondary structures and sub-systems (panel sheets, bulk-
heads, profiles, instrument enclosures, etc.), while GF-PCMs are used
for structural materials such as fittings, support, shrouds, ducting, an-
tenna enclosures and reinforcement laminates. Even if the parameters
of gaseous releasing are not negligible, the use of such composites
(especially in positions subjected to low/medium temperatures) is
generally enabled in view of not-harmful outgassing constituents and
location far from sensitive items, as in satellites assembling. KF-PCMs
are popular materials in spacecraft design and realization, where are
commonly used as support materials and shielding covers: that means a
higher level of danger from Kevlar outgases with respect to other ma-
terials used away of sensitive components, since the closeness to ele-
ments that need to be isolated.
OTF test and FT-IR findings thus establish the hand lay-up manu-
facturing as effective process to produce feasible CF-PCMs and GF-PCMs
(these latter under reserve about the specific allocation/functionality)
for aerospace application, while it should be rejected for KF-PCMs
fabrication, at first instance. Referring to the exceeding outgassing rates
provided by GF- and KF-based materials, a thermal pre-conditioning
treatment was carried out on the naked textiles in order to evaluate the
possibility of considering low-cost/commercially available PCMs for
employment in thermal-vacuum environment. A baking cycle was ap-
plied by heating GF and KF fabric sheets at 80 °C for 6 h in inert at-
mosphere, followed by keeping in dry-vessel (RH 0%) at room tem-
perature for 24 h before the resin impregnation and the composite
manufacturing; finally, as-prepared samples – GF*-PCM and KF*-PCM –
were tested in OTF by following the same procedure adopted for the un-
treated materials. As reported in Table 1, both composite typologies
present a significant lowering of outgassing rate parameters. In parti-
cular, fiberglass composite CVCM values fall within standard accep-
tance range, whit a related RML < 1% (that is a limit often adopted as
minimum tolerance requirement, less restrictive than TML < 1%) in-
dicating the prevalent content of water vapor in the released outgases.
Kevlar composite main parameters decrease by 30–40%, as evidence of
the cleaning effectiveness of thermal fibers pre-treatment; nevertheless,
the outgassing rates are still oversized to consider such kind of
R. Pastore, et al.
Fig. 4. Schematic representation of outgassing flux during an OTF test.
manufactured composite for actual applications. FT-IR analysis of the
treated materials suggests the formation of oxidation products; in par-
ticular, mean peaks lowering and shifting in KF*-PCM spectrum
(around 2900 and 800 cm−1, dashed bottom curve in Fig. 3 plot) may
be ascribed to the partial substitution of N–H group in the treated KF as
well as to an improved fibers/matrix interfacial adhesion.
The outgassing criticality of surface contamination may be eval-
uated by analyzing the relationship between CVCM and VWR para-
meters. A simplified schematic of the physical dynamics occurring
during OTF test provides a further evaluation of the obtained results,
based on that the overall mass loss can be classified into ‘non con-
densables’ and ‘condensables’ fraction, this latter being defined and
characterized herein as matter capable of condensing on a collector
kept at a temperature of 25 °C. In Fig. 4, without loss of generality, the
outgassing stream is distributed into four contributes:
α – mass % of water vapor not condensed onto the collector
β – mass % of other than water vapor (potentially harmful) not
condensed onto the collector
γ – mass % of water vapor condensed onto the collector
δ – mass % of other than water vapor (potentially harmful) con-
densed onto the collector
By definition, the following equalities hold:
TML  = α + β + γ + δ
Fig. 5. Quantitative analysis of the condensable matter outgassed from PCMs during OTF test.
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Acta Astronautica 170 (2020) 466–471
CVCM  = γ + δ (1)
whereas, assuming that samples recover the full pristine aqueous con-
tent after re-hydration step:
RML  = β  + δ
VWR  = α + γ (2)
As a matter of fact, for the above considerations the quantity δ may
be considered as a trial index of effective harmfulness. A further as-
sumption is needed to estimate such parameter: taking the standard
CVCM threshold (< 0.10%) as hint, the worst hypothesis of moisture
condensation, coupled to (1)–(2) relationships, gives
γ ≤ 0.1 × α → δ~ CVCM − (0.1×VWR) (3)
In Fig. 5 the values of δ calculated from OTF results, as well as the
graphical rates between harmful and total condensable amount are
given. In this framework, beyond the expected good working by CF-
PCM, the improved behavior of treated fiberglass PCM is assessed by δ
value of 0.071%, well below the condensation standard threshold; even
if effective in condensable decreasing, instead, the treatment of Kevlar
fabric is not sufficient to reach acceptable values of outgas condensa-
tion. The here introduced rate δ/CVCM may be helpful for a quantita-
tive estimation of condensable harmfulness, especially in those case
where single CVCM evaluations do not give clear indication of material
acceptance or rejection. Based on the obtained results, it can be es-
tablished that materials which have this index below or around 0.5 (as,
in this case, CF- and GF*-PCMs) can be considered suite for application
onto spacecraft surfaces, while should be avoided (or, at least, deeply
screened) otherwise.
4. Conclusions
Conventional fiber-reinforced polymeric composite materials were
manufactured by facile time/cost saving procedure and tested by means
of certified outgassing experimental set-up, in order to investigate their
behavior at high temperature/ultra-high vacuum conditions typical of
LEO space environment. The performed characterization was aimed at
assessing the detrimental effects of thermal-vacuum on the composites,
in terms of both mass loss due to gas releasing (which affect the
structural performance of materials themselves) and amount of re-
condensable matter (which is responsible of nearby surfaces con-
tamination issues). Carbon fiber composite proved to be efficient, since
R. Pastore, et al.
the measured outgassing rate parameters fall within the standard
thresholds usually adopted as acceptance criteria in space materials/
processes selection. Fiberglass composite revealed outgassing slightly
exceeding the limits; using this material in thermal-vacuum conditions
should be deeply screened, most of all with respect to the specific
functionality scheduled by space mission protocol. Kevlar reinforced
polymeric material showed the worst performances, with total mass
loss and collected volatile condensable amount well above the standard
requirements. Infrared spectroscopy analysis was performed in order to
gain knowledge about the chemical nature of the outgassed species:
carbon and glass fiber-based materials are believed to release mainly
not critical gases such as water vapor and carbon/nitrogen oxides,
while the presence of potentially harmful oily and plasticized volatile
content may be significant in the adopted Kevlar fabric reinforced
composite. A thermal pre-conditioning cycle was performed onto pris-
tine fibers with the aim to improve fiberglass and Kevlar composites
outgassing response; the treatment effectiveness was also evaluated by
introducing a schematic modeling of outgassing test dynamics, able to
discriminate the products of condensation over collectors. Treated fi-
berglass composites showed outgassing parameters below the standard
threshold, thus validating the entire procedure for realizing fiberglass-
reinforced materials suite for application in LEO thermal-vacuum con-
ditions. Outgassing rates remarkable lowering was also measured for
treated Kevlar fabric composites, even if still exceeding the safe-limits.
The proposed facile method thus sounds to be un-effective for manu-
facturing aramid-reinforced composites to be used in space environ-
ment; more refined technological routes – or mitigation techniques,
such as application of protective coating and shielding to protect
against or remove residual, process and handling contaminants – are
required for the processing of such materials to withstand harsh
thermal-vacuum conditions.
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