Materials Sciences and Applicatio ns, 2011, 2, 1399-1406
doi:10.4236/msa.2011.210189 Published Online October 2011 (
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers
Reinforced Glass Ceramic Matrix Composites
upon Oxyacetylene Torch Exposure
Julien Beaudet1, Jonathan Cormier1, André Dragon1, Magali Rollin2, Guillaume Benoit1
1Institut Pprime, Centre National de la Recherche Scientifique, Ecole Nationale Supérieure de Mécanique et d’Aérotechnique,
Université de Poitiers, Département Physique et Mécanique des Matériaux, ENSMA, Futuroscope Chasseneuil, France; 2Pyromeral
Systems S.A., Barbery, France.
Received August 16th, 2011; revised August 26th, 2011; accepted September 3rd, 2011.
The ablation properties of two laminated composites, having both a glass ceramic matrix and different kinds of fibers (C
or SiC) with the same architecture, are evaluated and compared. Ablation tests are performed using an oxyacetylene torch
on samples having two different thicknesses. Mass loss and ablation depth are measured after flame exposure. The results
obtained show that the decomposition of SiC fibers during t h ermal exposure has a si gni fi cant i mpact on abl ati on behavi or.
Oxidation of SiC produces a liquid SiO2 film at the top of the material during ablation. This leads to an improved ablation
resistance compared to the glass ceramic matrix/C composite, especially in case of successive flame exposures where the
SiO2 fil m consumes a substantial f ract ion of the heat flow during i ts liquefacti on upon re-heat ing.
Keywords: Fiber, Ablation, High-Temper at u re Propert i es
1. Introduction
Ceramic matrix composites are widely used for many
engineering applications concerning severe loading con-
ditions including ballistic context or re-entry of space
vehicles. For such applications, the material degradation
mainly results from aerodynamic impact involving in-
tense mechanical and thermal loading. Thermal protec-
tion is an essential factor of structural integrity for a
spacecraft vehicle during re-entry phase. High thermal
resistance of the corresponding material is required
against short intense thermal and mechanical load.
Moreover, regarding flying structures, one of the pri-
mary design criteria is the mass gain. In this respect, in-
creasing ablation resistance for protective structures of
limited mass is an obvious technical challenge for space-
craft–related research and development [1].
In this context, strong research effort has been devoted
to the study of ablative materials [2-5]. In conjunction
with the mass gain imperative, the thermal protection
systems employing composite materials have been de-
veloped. One feature of technological advances has been
a substitution of polymer ablators (resol phenolic com-
posites) by Ceramic Matrix Composite (CMC) ablators
(having high thermal resistance). In such a way, Ceramic
Matrix Composite (CMC) ablators have been introduced
as coating protection materials and their thermal behavior
has been extensively studied [1]. However, in addition to
their relatively high cost, one of the major problems of
the CMC/carbon based protection systems is their poor
oxidative behavior: under exposure to a hot oxidative gas,
a notable bulk material mass loss is observed due to
chemical reactions with oxygen and water vapour. These
phenomena have been reported by many authors [6-10]
and more reliable carbon based systems have been
searched for.
Chen et al. report on the ablation properties of carbon
matrix reinforced carbon composite (C/C) exposed to
oxygen/ethanol hot combustion mixture [2]. In the con-
text termed “thermo-chemical ablation” by the authors,
ablation rate is increasing with the Oxygen/Ethanol ratio.
Chen et al. [9] examine ablated C/SiC samples after
oxyacetylene torch exposure. Scanning electron micro-
scope (SEM) observations indicated white SiO2 dross
produced by chemical recombination and oxidation of
SiC in the ablated area. Several other authors [7] pointed
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon
Oxyacetylene Torch Exposure
out the generation of new specific microstructures during
ablation processes. However, scarce work is available on
the ablation performance correlated with the above men-
tioned observations.
During the last decade, the requirements for compos-
ites having the same (or closely same) high temperature
mechanical performances under fire exposure and with a
low environmental impact during the elaboration process,
lead to the development of composites with ceramic ma-
trix derived from geopolymer systems. Few authors have
investigated the fire behavior of this new category of
high performance composite [11,12] with specific high
temperature tests.
In the present work, the ablative properties of two
composites with the same glass ceramic matrix are stud-
ied and an approach is attempted to show the advantages
of a SiC Reinforced Composite (SiRC) compared to a
Carbon Reinforced Composite (CRC). The correspond-
ing specimens are exposed to oxyacetylene flame. Weight
loss and ablation depth are measured after each test.
SEM observations provide indications regarding the ki-
netics of material degradation. The ablation test results
are finally analyzed as a function of the thermal loading,
and degradation mechanisms are proposed.
To our best knowledge, this is the first time that glass
ceramic composites derived from geopolymer systems
are characterized under very high temperature ablative
2. Experiments
2.1. Specimen
Two kinds of composite materials are tested. The first
one (denoted as SiRC in the following of the artcile) is
reinforced by silicon carbide fibers while the other one
(denoted as CRC) is reinforced by carbon fibers. Both
have a glass ceramic matrix. Samples were supplied by
PYROMERAL SYSTEMS SA, in the form of 50 × 50
mm2 plates with different thicknesses: 5 mm for CRC
(PyroKarb® family), 2.5 and 5 mm for SiRC (PyroSic®
Specimens are 2D laminated twill woven. The Pyro-
Sic® composite (SiRC) is a silicon-carbide-fiber-rein-
forced glass ceramic composite, with a 42% fiber volu-
metric ratio and 12% porosity. It has been developed for
thermostructural applications at temperature up to 1000˚C
The PyroKarb® composite (CRC) is a carbon-fiber-
reinforced glass ceramic composite, with a 47% fiber vo-
lumic ratio and 23% porosity. It has been developed for
thermostructural applications at temperature up to 500˚C.
The matrix of these composites is a glass ceramic in
the system K2O-SiO2. It is obtained by impregnating the
fiber with an inorganic polymer. During the thermoset-
ing, a 3D-network of oxide molecules is formed. The
final composition and microstructure of the glass ce-
ramic matrix is obtained from an adapted thermal treat-
2.2. Characterization
Thermogravimetric analysis (TGA) was performed using
a TA Instruments SDT 2960 device. The temperature
was varied from ambient to 1200˚C under air using a
heating rate of 10˚C·min 1.
The morphology and microstructure of samples before
and after ablation tests were examined by scanning elec-
tron microscopy (SEM) using a JEOL 6100 microscope.
Both transverse sections and top (i.e. normal to the ab-
lated surface) views were used to characterize the sample
microstructures after ablation exposure. Optimal SEM
operating conditions were obtained using an acceleratory
tension in the range 5 kV - 12 kV, depending on the
sample type.
2.3. Ablation Conditions
The ablation tests were performed using an oxyacetylene
torch based on the ASTM E 285-80 standard. This kind
of test is widely used for the characterization of the abla-
tion resistance of materials [5,9,10,14,15]. An air tight
box was designed specifically for experiments. An elec-
tric linear actuator was used to move the sample under
the flame. Sapphire glasses allowed measuring the tem-
perature of the in-ablation surface using dual wavelength
pyrometer during tests. This kind of radiometer takes into
account the emissivity modification of the material dur-
ing ablative exposure. The rear face temperature was
measured with a K Type (chromel-alumel) thermocouple.
Signals were recorded by an analogic acquisition card
and transferred to a computer.
The torch was a blowpipe FAREL O/Si with an ex-
haust diameter of 1.1 mm (n˚4). Pressure levels of O2 and
C2H2 were respectively set to 2 and 0.25 bar. The corre-
sponding flow rates were 355 nl·h1 (O2) and 125 nl·h1
(C2H2). This set-up produces approximately a 3300 K
oxidative flame at the nozzle tip and a maximum heat
flow of 5.40 × 106 W·m2 at the sample surface.
An example of the surface temperature evolution re-
corded during a 30 s exposure at maximum heat flow is
presented in Figure 1. It is observed that the surface
temperature remains almost constant within a 2350 -
2500 K range once the maximum temperature is reached.
Two kinds of ablation tests were performed: either
simple exposure (SE) where ablation time varied from 2
to 30 s or multi-exposure (ME) where the exposure se-
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon 1401
Oxyacetylene Torch Exposure
Figure 1. Surface temperature recording for a 30 s ablation
test of a CRC composite.
quence was split into two or more events for a fixed total
time. The total time was set to 20 s while the cooling
time is set to 1 minute between each exposure. The tested
sequences were: 2 × 5 s + 10 s, 2 × 10 s and 15 s + 5 s.
The surface degradation was also recorded during ab-
lation tests using a high resolution camera and specific
filters to avoid any damage of the CCD camera due to
high radiation of the in-ablation surface.
After ablation exposure, samples were analyzed as
Mass of the sample was measured with a digital bal-
ance whose resolution is ±0.5 × 104 g and compared
to its initial mass before ablation.
Ablation depth was evaluated by a mechanical pointer
whose resolution is 1 µm. The difference between the
initial surface height and the bottom of the ablated
area was systematically quantified
These two quantitative criteria account for volumetric
and surface ablation [15] respectively.
3. Results
3.1. TGA Experiments
Figure 2 plots the mass evolution relative to the initial
mass (i.e. actual mass/initial mass) as a function of tem-
perature. A progressive and limited (1% at the maximum)
mass loss is observed until a plateau is reached at ap-
proximately 750 K for both materials. Afterwards, a
mass gain is observed until 1473 K.
Both materials exhibit the same TGA behavior except
in the last part of the curve (i.e. for a temperature over
1300K) where the mass gain is more pronounced for the
Figure 2 shows that a mass gain is observed for both
materials in the temperature range 700 - 1470 K. For
temperature lower than in the ablation tests, the two
composites exhibit the same behavior.
Figure 2. TGA curve for SiRC and CRC under air atmos-
3.2. Ablation Tests
Figures 3 and 4 present the mass loss and the maximum
ablation depth as a function of ablation time after each
Simple Exposure (SE) at a surface temperature of 2500
K for 5 mm thick samples.
For each material, the mass loss follows a linear evo-
lution between 5 and 30 s (Figure 3). The CRC appears
to be more sensitive to mass loss compared to SiRC for
the same ablation conditions: the mass loss rate is clearly
higher for the carbon reinforced composite. The respec-
tive values are 2 × 103 g·s1 for SiRC compared to 1.5 ×
102 g·s1 for CRC. The degradation rate is thus nearly 10
times greater for the CRC.
For example, after 10 s, CRC looses approximately
0.15 g and for the SiRC, the weight loss is 0.025 g. After
25 s the gap between the corresponding weight losses
After evaluating the weight loss, the ablation depth is
checked: the corresponding results are shown in Figure 4.
As for weight loss, the variation of ablation depth is lin-
ear with respect to time for the two composites (from 5 to
45 s). The CRC has approximately 40% deeper ablation
compared to SiRC. Erosion rates are respectively 4 × 102
mm·s1 and 7 × 102 mm·s1 for SiRC and CRC composi-
The SiRC exhibits better ablation properties than CRC,
both in terms of mass loss and ablation depth. For similar
fiber architecture and matrix, the SiC reinforcement of-
fers better resistance to high temperature exposure than C
reinforcement under ablation conditions with an oxya-
cetylene torch.
3.3. Ablation Microstructures
Figure 5 presents SEM microstructures for both materi-
als after a 20 s/2500 K exposure. The SiRC bulk appears
to be more porous than the CRC. The proportion of ma-
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon
Oxyacetylene Torch Exposure
Figure 3. Mass loss versus ablation time for “single” expo-
sure for 5 mm samples.
Figure 4. Ablation depth versus ablation time for 5 mm
trix in the heat affected zone is clearly different from the
virgin material for the SiRC composite. Delamination is
apparent in this area for SiRC and glass is formed in the
center of the ablation region. It is supposed that the liq-
uefied matrix has risen up by a capillarity mechanism to
the top of the material.
In summary, SiRC seems to be more affected by
volumetric ablation compared to CRC; the latter has a
lower porosity compared to SiRC.
Figure 5 also reveals droplets at the top of the CRC
material. It is not the same glass structure as that ob-
served for the SiRC composite but it seems likewise to
be composed of glass. In fact, EDX measurements (not
presented in this article) revealed that those droplets are
mainly composed of Silicon and Oxygen. These droplets
arise from the thermo-oxidation of the glass ceramic ma-
Videos recording during ablation highlight the very
different ablative behavior of the materials. Some snap-
shots taken from the ablation video recording are pre-
sented in Figure 6. It is observed in Figures 6(a), 6(c)
that the two composites have very different ablation be-
Figure 5. Cross section microstructures of SiRC (a) and
CRC (b) after single 20 s exposure at 2500 K.
havior in the very first moments (1 - 2 s) of ablation ex-
posure. The SiRC melts with bubble formation whereas
the CRC seems to volatilize accompanied with the for-
mation of droplets.
These marked differences between CRC and SiRC
during ablation reside in the occurrence of bubbles and
the liquid material in the centre of ablation during fire
exposition for the SiRC.
When increasing the ablation time, no liquid phase is
observed at the CRC surface while the SiRC surface ap-
pears as a boiling liquid as seen in Figures 6(b) and 6(d).
These observations confirm the presence of a liquid film
at the surface of material during ablation.
3.4. Influence of Thickness on Ablation
Properties of SiRC
The ablation resistance of the CRC is mainly controlled
by the thermo-oxidation rate of the fibers and of the ma-
trix while ablation resistance of SiRC is controlled by
more complex state transformations which will be dis-
cussed in Section 4.
In his numerical study, Staggs [16] reports that the ab-
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon 1403
Oxyacetylene Torch Exposure
Figure 6. In-ablation area after 1 s under the torch for SiRC
(a) and CRC (c), similar observations after 5 s of exposure
for SiRC (b) and CRC (d).
lation rate is influenced by the thickness of the structure.
To evaluate the effect of the sample thickness, the abla-
tion tests were conducted on the SiRC for two different
thicknesses (5 and 2.5 mm). The corresponding results
are presented in Figures 7 and 8.
The linearity of the mass loss as a function of time is
still observed for both types of samples, with a higher
mass loss rate for the 2.5 mm SiRC composite samples
than for the 5 mm thick. For a half thickness sample, the
mass loss rate is approximately 5 times greater.
For the 5 mm thick SiRC composite samples, it ap-
pears that the ablation degradation is non-linear: in the
first seconds of exposure, an apparent mass gain and
thickness increase are obtained, see Figure 8.
The evaluation of the ablation depth after exposure
showed the same general trend. The influence of the ini-
tial sample thickness is more significant for the ablation
depth than for the mass loss.
After an initial non-linear regime, the ablation behave-
ior seems to display more or less linear degradation dur-
ing the exposure. The negative values reported in the first
5 seconds correspond to the void growth and the glass
formation observed in the SEM photograph (Figure 5).
3.5. Influence of Sequence of Exposure
For exposure time under 5 s, the SiRC reinforced com-
posite showed a mass gain and surface expansion: this is
obviously connected with non linear ablative behavior
observed in Figures 7 and 8.
A specific test consisting in sequential exposures (ME
5 mm
2.5 mm
Figure 7. Mass loss for two different SiRC composite thick-
5 mm
2.5 mm
Figure 8. Ablation depth for two different SiRC composites
tests) was then specified to get a better understanding of
this phenomenon and of its influence on the ablation
properties. Mass loss and ablation depth in case of ME
tests are presented in Figures 9 and 10, respectively.
It is observed that when the number of exposure se-
quences decreases, the ablation depth and mass loss rise
up for SiRC while CRC remains almost insensitive to the
exposure sequence. It can only be noted a very slight
mass loss increase with the sequence length increase for
For SiRC, there is a link between the number of expo-
sure sequences and the degradation. For many short se-
quences under hot gases, degradation is smaller than for
the same time using one global exposure.
4. Discussion
The ablative properties of two composites having the
same glass ceramic matrix and the same architecture but
different fibers are studied. The nature of fibers has been
identified to have a deep impact on the ablation resis-
tance, especially in case of multi-exposures where SiRC
exhibits superior ablative properties.
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon
Oxyacetylene Torch Exposure
Figure 9. Mass loss of SiRC under multi-exposure sequen-
ces for estimating ablation behavior under complex thermal
Figure 10. Ablation of SiRC under multi-exposure sequen-
ces for estimating ablation behavior under complex thermal
The origin of such differences in ablation resistance is
addressed in the first part of the discussion below while
the second part is aimed at summarizing the ablation
mechanisms of these composites.
4.1. Differences in Ablation Resistance between
SiRC and CRC
The SiRC composite has been identified to be a better
ablator than CRC under 2500 K oxidative ablation condi-
tions. This result is not obvious based on TGA results
which were performed until 1473 K (Figure 2).
In fact, both materials exhibit a very similar mass loss
behavior in the investigated TGA temperature range, ex-
cept for the highest temperatures (T > 1300 K) where the
SiRC was found to have a higher mass rate increase com-
pared to CRC. It is therefore clear that the difference in
ablative resistance of both materials arises from chemical
reactions encountered in the 1300 - 2500 K range, and
especially, the oxidation of the materials compounds.
Many authors reported that for high temperature and
oxidative conditions, the solid carbon begins to react
with oxygen at 800 K. Many other species interact with
solid carbon during exposure with the following chemi-
cal reactions [2]:
 
2gs 2g
 (1)
 
2g sg
 
 
2g sg
 
gs g
 (5)
 
 
The SiC based composites exhibit a better oxidation
resistance compared to the carbon reinforced composites
since, as it has been shown, the SiC reacts with oxygen to
form a protective SiO2 glass film at the top surface of the
material and in the interbundle pores [3]. SiO2 is a well
known effective diffusion barrier against the inward dif-
fusion of oxygen. When surface temperature is close to
2000 K, liquid SiO2 flows and plugs the cracks and pores
in the surface, thus providing a sufficient oxidation pro-
tection due to its very low oxygen diffusivity, reported to
be 3.5 × 1014 m2·s1 in literature [5].
In our experiments, the SiO2 liquid phase is clearly
observed during ablation (Figure 6(b)). This mixture is
only observed at the top surface of the SiRC due to the
decomposition of fibers while CRC exhibits Si rich
droplets (evidenced by EDX measurements not shown
here) produced by the glass matrix decomposition.
Another interesting point regarding the beneficial ef-
fect of the SiC degradation into a SiO2 liquid film is ob-
tained for short timespan exposures at 2500 K (t < 5 s). A
mass gain and a thickness increase are observed due to
SiO2 film formation (Figures 3 and 4). Biamino [4] de-
scribed this mass gain/mol as 50% mol. (40.10 g·mol1
SiC and 60.08 g·mol1 SiO2) which overcompensates the
mass losses due to CO release by Equations (1), (2), (4),
(5), (7). In this case the overall procedure is called “pas-
sive oxidation” of the SiC composite. If the oxygen reach-
es the silicon carbide fibers through cracks or because of
the failure of the protective layer, then the overall proce-
dure is called “active oxidation” of the SiRC and is fol-
lowed by a mass reduction of the sample [17].
For short exposure time of SiRC, mass measurements
provide evidence for this hypothesis while for longer
exposure, the heat and oxygen species released by oxya-
cetylene torch diffuse through the composite and the ac-
tive oxidation begins (exposure time > 5 s). The reaction
Copyright © 2011 SciRes. MSA
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon
Oxyacetylene Torch Exposure
Copyright © 2011 SciRes. MSA
2SiC 3O2SiO2CO 
below shows the SiO2 formation [4,8,10]: produce liquid SiO2 in impacted area. Voids appear in
the resulting volume (volumetric ablation). This phase
change is endothermic. A part of the inflow is absorbed
by this reaction. Fused SiO2 protects from the oxidation
and absorbs energy. This is the first step of ablation: the
passive oxidation.
 
22lg (8)
The SiO2 film is beneficial for all the investigated SE
conditions probably due to the above mentioned low
oxygen diffusivity of SiO2(l) but the most spectacular
effect of the SiO2 formation is observed in our experi-
ments in case of multi-exposures (ME) tests.
The second step begins when the SiO2 temperature rises
to the vaporization threshold. On the one hand the heat is
driven in the bulk and on the other hand, fibers begin to
react with hot gases and the material loses mass. Upon
cooling, SiO2 is solidified to form an amorphous glass.
For a given total ablative time of 20 s, an increase in
the number of torch exposure sequences (i.e. a decrease
of the average exposure time) leads to an ablation depth
which can be divided by 10 (Figure 10) and dwindling in
mass loss, reaching even a mass gain (Figure 9). In con-
trast with the SiRC the CRC composite behavior remains
almost unaffected by the ablation sequence under the
investigated conditions. This much more pronounced
effect of the SiO2 film formation in ME experiments
compared to SE tests can be explained by the SiO2(l)
SiO2(s) transformation upon cooling between exposures
and the SiO2(s) SiO2(l) transformation upon re-heating.
Figures 7 and 8 show the effects of different thick-
nesses for the SiRC composite. The mass loss is clearly
influenced by the size of the samples. These results con-
firm the analysis of Staggs [16]. For a thinner sample, the
influence of thermal resistance of air in rear face is more
effective. The heat is trapped in the material due to the
low thermal coefficient of natural convection in rear face.
The heat flow conduction is strongly limited. As a result,
the local temperature increases rapidly. The degradation
occurs in a shorter time than for a thick material with high
diffusion ability. For a thin plate, the instantaneous heat-
ing leads earlier to active oxidation than for a thick one.
In fact, SiO2(s) is an even more efficient diffusion bar-
rier and the solid liquid phase change (at T 1750 K
± 75 K [18]) is endothermic, thus, leading to a reduced
net heat flow received by the material and finally to a
reduced ablation.
The last kind of test conducted is ME (multi-exposures)
test. Degradation decreases with an increase of the num-
ber of exposure stages. For a short exposure period, a
passive oxidation produces an amorphous solid glass
during cooling. This glass has a high melting point and
so, during the subsequent torch exposure, the material is
protected by this SiO2 coating. For the same number of
stages, degradation is driven by a time of the longest ex-
posure. A longer time under the torch produces a larger
heat-affected zone and so, a larger reaction zone with
oxidative species.
4.2. Degradation Mechanisms
The experiments performed in this study allow us to
propose a scenario of the degradation mechanisms for the
SiRC composite (Figure 11).
Once the material is exposed to hot gases (T 3000 K)
the impacted area is instantaneously heated. The SiC
reacts with the hot oxidative gases. SiO2 appears result-
ing from SiC oxidation. A capillarity mechanism leads to
Figure 11. Degradation mechanisms of SiRC composite during ablation.
Ablation Properties of C Fibers and SiC Fibers Reinforced Glass Ceramic Matrix Composites upon
Oxyacetylene Torch Exposure
5. Conclusions
The carbon-reinforced glass ceramic matrix composite
exhibits a poorer ablation resistance under oxyacetylene
torch compared to the SiC reinforced one. This superior
ablation resistance of SiC glass ceramic matrix has been
evidenced for either of torch exposure tests (simple and
sequential) where the difference between both materials
is even enhanced. This superior ablation resistance of
glass ceramic matrix/SiC composite results from the
formation of an SiO2 liquid film whose melting is endo-
thermic at temperature above 1600 K, hence reducing the
net heat flow received by the in-situ SiO2 coated com-
6. Acknowledgements
The authors gratefully acknowledged Christelle Roudault
(LACCO, UMR CNRS 6503) for her help in the TGA
experiments. Thanks to Damien Marchand for technical
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