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Composites: Part A 30 (1999) 429437

Recent developments in fibers and interphases for high temperature


ceramic matrix composites
Richard E. Tressler*
Department of Materials Science and Engineering, The Pennsylvania State University, University Park, PA 16802, USA

Abstract
The long term durability of CMCs is limited by two factors: (1) creep and rupture of the fibers, and (2) environmental degradation of the
constituents, primarily in the nonoxide composites. Oxide CMCs are limited by the creep resistance of the fiber at this stage of development
and by interphase concepts that are not yet mature. Nonoxide fibers have been developed with excellent creep resistance relative to oxide
fibers, but oxidation of the interphase and the interface, particularly at intermediate temperatures, causes embrittlement of these composites.
This effect is particularly severe when matrix cracks are present and under cyclic loading conditions. 1999 Elsevier Science Ltd. All rights
reserved.
Keywords: A. Ceramic fiber; A. Ceramic matrix composites (CMC); B. Interface/interphase

1. Introduction
Ceramic matrix composites have the potential to provide
unique combinations of properties at high temperatures, e.g.
high strength, creep resistance, toughness and environmental stability. The properties of the fibers and the interfaces or
interphases between the fibers and matrix are recognized as
the critical elements in achieving the flaw tolerance or notch
insensitivity that distinguishes these materials from monolithic ceramics. Outstanding properties have been demonstrated for CMCs, particularly silicon carbide fiber/silicon
carbide matrix composites (SiC/SiC) with either carbon or
BN interphases. Composite properties have been demonstrated for oxide composites, particularly Al2O3/Al2O3
with tailored interphases, but the database is very limited
in this case.
The long term durability of CMCs is limited by two
factors: (1) creep and rupture of the fibers, and (2) environmental degradation of the constituents, primarily in the
nonoxide composites. Oxide CMCs are limited by the
creep resistance of the fiber at this stage of development
and by interphase concepts that are not yet mature. Nonoxide fibers have been developed with excellent creep resistance relative to oxide fibers, but oxidation of the interphase
and the interface, particularly at intermediate temperatures,
causes embrittlement of these composites. This effect is
particularly severe when matrix cracks are present and
under cyclic loading conditions.
* Corresponding author. Tel.: 1-814-865-7961; fax: 1-814-865-2917.

In this paper the most recent developments in nonoxide


and oxide fibers are reviewed, particularly as they affect the
high temperature properties. In previous reviews, the
general performance requirements for high temperature
fibers were described, and the state-of-the-art at that time
in nonoxide and oxide fibers relative to these requirements
was reviewed [1,2]. Developments in interphases for more
durable SiC/SiC composites are reviewed and promising
interphases for oxide composites are discussed.

2. Developments in fibers
Ceramic fibers for high temperature applications can be
grouped as nonoxide fibers or oxide fibers. The nonoxide
fibers of interest are primarily based on silicon carbide
although amorphous or nanocrystalline SiBNC fibers
with excellent high temperature properties have recently
been introduced. The oxide fibers are primarily alumina
based, but the best properties in polycrystalline fibers have
been realized with multiphase fibers (e.g. alumina plus
mullite). The nonoxide fibers of most interest are either
chemical vapor deposited (small diameter fibers have not
yet been achieved) or polymer-derived with complex curing
and pyrolysis steps to achieve the end properties. The strongest polymer-derived fibers have very small (nanocrystalline) b -SiC grains with carbon and an amorphous phase
which results in low elastic modulus and high strains to
failure (1%). The creep resistance is improved by
increasing the b -SiC grain size and reducing the oxygen

1359-835X/99/$ see front matter 1999 Elsevier Science Ltd. All rights reserved.
PII: S1359-835 X( 98)00 131-6

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R.E. Tressler / Composites: Part A 30 (1999) 429437

Fig. 1. Tensile strength of various silicon carbide fibers [3].

level to very low levels (0.5%) which results in higher


modulus and lower strengths, in general.
2.1. Nonoxide fibers
The fast fracture strength as a function of temperature for
some of the most recently developed nonoxide fibers is
shown in Fig. 1 [3]. The improvement in the low oxygen
content in Hi-Nicalon compared to the Nicalon fiber is
apparent. The superior strengths of the CVD SiC fibers at
elevated temperatures are also clearly demonstrated. Other
low oxygen content polymer-derived fibers based on nanocrystalline SiC, e.g. the Tyranno LOX family and the
University of Florida 3M fiber, are expected to show similar
fast fracture strengths at high temperatures and are expected
to show behavior similar to the Hi-Nicalon fibers.
The Dow Corning Sylramic fiber, which is a boron and
titanium doped, polymer-derived fiber which has been fully
crystallized to a near stoichiometric b -SiC material, is
expected to exhibit good strength retention at high temperature although published data is not available. The

Fig. 2. Tensile strength of SiC fibers after heat-treatment in Ar for 1 h [4].

Fig. 3. Tensile strength of SiC fibers after 10 h exposure in argon [5].

carborundum sintered a -SiC fiber, which is no longer available, showed fast fracture strengths at 1400C of 90% of
its room temperature strength. Thus, it is expected that the
fully crystalline, stoichiometric SiC fibers will show very
little strength decrease between room temperature and
1400C.
The effect of aging at high temperatures on the properties
of these fibers is important because the fabrication conditions are generally severe and the eventual service conditions involve high temperatures. Fabrication conditions are
simulated by aging in inert or reducing ambients while
service conditions can involve oxidizing, inert and reducing
conditions. Fig. 2 compares the retained strength of the
LOX family of Tyranno fibers to Nicalon after aging in
argon for 1 h [4]. Fig. 3 compares the new Hi-Nicalon and
developmental near stoichiometric Hi-Nicalon S to Nicalon
after high temperature exposures in argon for 10 h [5].
Clearly, the reduction of oxygen content and higher pyrolysis temperatures yield fibers which are much more stable
to the degradation by SiO and CO evolution from the fibers.
The Sylramic fiber is even more resistant to degradation
during aging in argon at high temperatures [6].
The oxidative degradation at 1400C is illustrated for the

Fig. 4. Tensile strength of SiC fibers after 1673 K exposure for 10 h in dry
air [5].

R.E. Tressler / Composites: Part A 30 (1999) 429437

Fig. 5. Tensile strength of fibers after heat-treatment at 1273 K in air [4].

Nicalon family of fibers in Fig. 4, for the Tyranno family of


fibers at 1000C in Fig. 5, and for the Sylramic fiber at
1200C in Fig. 6. All of the SiC-based fibers show loss of
strength at room temperature after oxidation; however, no
direct comparison of this property under identical
conditions has been performed.
The recently reported amorphous SiBNC fiber being
developed by Bayer shows promise for use at high temperatures. For example, excellent thermal stability has been
reported such that the fiber remains amorphous after extensive heat treatments up to 1800C in an inert environment.
The Bayer fiber is also unusually resistant to oxidation (for a
nonoxide fiber), producing only a 1 mm thick oxide film
after 48 h exposure to air at 1500C. Equally interesting,
is the hexagonal boron nitride (h-BN) interlayer that
forms under the SiO2 film in-situ. This h-BN interlayer
appears to act as a crack deflector in much the same way
as a CVD BN film [7]. However, the remarkable strength
retention and creep resistance of the Bayer fiber is neither
verified nor understood.
The recent developments which have resulted in low
oxygen content polymer-derived fibers and near stoichiometric or stoichiometric SiC fibers have dramatically
improved the creep resistance of this group of fibers.
These results are captured in a composite figure using
bend stress relaxation (BSR) data by Nippon Carbon and

Fig. 6. Room temperature strength after aging SYLRAMIC fiber at 1200C


in dry air [6].

431

DiCarlo [5,8] (Fig. 7). Here, 1-h BSR test results as a function of temperature are presented for many of the commercially available and developmental fibers 1. In these results,
the Carborundum fiber has the highest creep resistance
(except for the annealed Hi-Nicalon type S); the Hi-Nicalon
S and the Dow Corning fiber follow. The highest ranked
production fiber is the Hi-Nicalon fiber.
Based on these results and extensive tensile creep tests on
as-received and annealed fibers of several types, certain
generalities emerge for a given class of SiC-based fibers
(e.g. polymer-derived versus sintered versus CVD). SiC
grain size and volume fraction control the creep resistance.
The composition and spatial locations and sizes of secondary phases also affect the creep behavior. For example, in
the Nicalon family, the Hi-Nicalon fiber is much more creep
resistant than the Nicalon fiber because the SiOC secondary phase is essentially replaced with turbostratic (nongraphitic) carbon. If the SiC grain size is increased by
annealing, the creep resistance increases. In fact, a 1 h,
1600C anneal in argon causes the Hi-Nicalon fiber to
approach the creep resistance of the Carborundum fiber
[9]. Increasing the volume fraction of b -SiC to near stoichiometry with a concomitant doubling of the grain size
drastically increases the creep resistance of the Hi-Nicalon
type fiber (Hi-Nicalon S versus Hi-Nicalon).
The Dow Corning and Carborundum fibers are comparable in terms of type of microstructure in the final product
except that the grain size of the Carborundum material is 3
10 times the grain size of the Dow Corning fiber. The resultant creep resistance scales as one expects for diffusional
creep. The change in creep rate of the CVD-SiC has been
quantitatively accounted for by grain coarsening effects on
the diffusional creep rate [10].
However, attempts to quantitatively rationalize the
observed creep rates across the various classes of SiC fibers
have remained elusive. For example, the creep rate of the
annealed Hi-Nicalon fiber is very similar to that of the
Carborundum fiber yet the grain sizes of the SiC grains
are different by a factor of 1020. The CVD b -SiC fibers
have grain sizes on the order of 410 times larger than the
Hi-Nicalon fiber but yet creep rates of 10100 times that of
Hi-Nicalon. The NASA-Lewis group has found that the
Sylramic fiber with lower boron content is more creep resistant but the effect has not been quantified.
Thus, the fundamental questions as to what controls the
creep rates of these SiC-based materials are still open. What
is the role of carbon, of solid solution dopants? Do the
stacking faults in b -SiC grains play a role? Is the a -SiC
microstructure intrinsically more creep resistant? These
effects need to be better understood.
1
The m value plotted in Fig. 7 is defined by m Ro/Ra where Ro is the
initial loop radius imposed on the fiber before thermal exposure and Ra is
the radius of curvature after thermal exposure during which the fiber creeps,
thus relaxing the imposed stress. The higher the m value is, the more creep
resistant is the fiber.

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R.E. Tressler / Composites: Part A 30 (1999) 429437

where the LarsenMiller parameter q is a function of fiber


rupture time (t), temperature (T) and effective rupture
activation energy (Q) (R is the universal gas constant):
q Q=2:3R Tlog t D:

Fig. 7. One-hour stress relaxation ratio of PCS-derived SiC fibers and other
polycrystalline SiC and Al2O3 fibers [5,8].

The literature on creep rupture and stress rupture (time to


failure at a given stress) is meager. Researchers at NASA
Lewis have done comparative stress rupture studies of the
various SiC-based fibers in air and argon [11]. In Fig. 8 these
data are presented for the Dow Corning, Carborundum, HiNicalon, and annealed Hi-Nicalon (1600C, 1 h, argon)
fibers. The fibers generally performed better in air except
for the annealed Hi-Nicalon where oxidation of internal
porosity is thought to accelerate creep failure. Rugg et al.
[12] have shown that failure of the Carborundum fiber at
these stress levels in the 0100 h time frame are due to slow
crack growth and not creep-induced damage. Although this
fiber has about 50% of the room temperature strength of the
other fibers, it has about the same 100 h rupture strength at
1400C as the other fibers.
Yun and DiCarlo [13] have characterized the high
temperature rupture strength of ceramic fibers with the
LarsenMiller formulation of thermally activated rupture

For the rupture of SiC and Al2O3-based fibers the activation rupture time parameter (u ) was observed to be constant
(u o) and independent of stress conditions, such that average
rupture strength (S) can be described as a function of only
the LarsenMiller parameter (i.e. S S(q)). Here, D
log(u o) 22 for the SiC and Al2O3 fibers in the high
temperature range where creep cavitation controls failure
(q 32 000 for Nicalon SiC fibers, q 20 000 for the
polycrystalline oxide fibers) [14].
Yun and DiCarlo have merged the slow crack growth
dominated regime and the creep generated flaw controlled
regime into a rupture plot for Hi-Nicalon using the q parameter as described above (Fig. 9). In this way the whole
stress rupture plot at various stresses and temperatures is
represented. Using this same approach the comparable
data for Nicalon, CVD SCS-6 and a small diameter CVD
SiC by Textron (Ultra-SCS) are presented with the curve for
the Hi-Nicalon data (Fig. 10). Over a significant range of
temperature and stress (starting at 1000C for 1000 h) the
Hi-Nicalon has superior performance to SCS-6. However,
the Ultra SCS has superior performance over the whole
temperature range.
It should be noted that the comparisons are based on
very small data sets, which represent relatively short
times. Longer term durability studies should be emphasized particularly with coated fibers and in oxidizing
environments. Rupture strength studies are needed for all
nonoxide fibers.

Fig. 8. Rupture strength of SiC fibers in air (open symbols) and argon (closed symbols) at 1200C (K) and 1400C (A) [11].

R.E. Tressler / Composites: Part A 30 (1999) 429437

433

Fig. 9. Thermal activation plot for Hi-Nicalon fast-fracture and rupture strength in air [14].

2.2. Oxide fibers


Earlier reviews by Tressler and DiCarlo [1,2] and recent
papers by DiCarlo and co-workers [11,15,16] have illustrated the limitations of these fiberstheir poor creeprupture resistance at high temperatures compared to the
nonoxide fibers. The most promising directions for
polycrystalline oxide fibers appear to be ternary oxides
such as yttrium aluminum garnet and composite fibers
such as the Nextel 720 fiber, an aluminamullite fiber. In
Fig. 11 the creep resistance of the developmental Nextel
720 fiber is compared to other polycrystalline oxide fibers
[17].
The Nextel 720 fiber has both a secondary phase and
elongated grains incorporated into its microstructure. The
(55 volume %) mullite is present primarily as needles

surrounding the Al2O3 grains (45 volume %). Thus, the


creep resistance of the Nextel 720 is better than other oxide
fibers. However, the use temperature under a 100 MPa load
(1% strain in 1000 h) is less than 1200C.
Yun and DiCarlo have compared the rupture behavior of
this new fiber to the Nextel 610 and the single crystal
sapphire fiber using the LarsonMiller parameter (Fig. 12)
[14]. Failure by creep-induced flaws (high temperature, low
stress region) and the slow growth of existing flaws (low
temperature, high stress region) are both included in this
plot. The multiphase Nextel 720 fiber is clearly superior
to the fine grain alumina.
The recent work of Goring and Schneider illustrates the
need to better understand the stability of this two-phase
microstructure [18]. They have shown that at temperatures
of 1300C and above grain growth results in lowered

Fig. 10. Thermal activation plots for average strength of as-produced SiC fibers [14].

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R.E. Tressler / Composites: Part A 30 (1999) 429437

Fig. 11. Creep rate of Nextel 720 compared to other commercial oxide fibers [17].

strength in heat treatment times of 2 h. Furthermore, the 2 h


heat treatment at 1300C caused an increase of the creep rate
by 60%.
2.3. Fiber coatings and interphases
The interface between the fiber and matrix must be a low
energy crack propagation surface so that matrix cracks
deflect at the interface, thereby providing damage tolerance.
Fiber coatings or interphases are used for this purpose and
also to protect the fibers during fabrication or from environmental attack during use. An interphase constituent can
develop in situ as in the classic case of Nicalon fibers in
glass-ceramics.

Since Nicalon fibers have been commercially available


for many years, coatings and interphase developments have
concentrated on nonoxide fibers. Carbon and BN have been
the only truly successful interphase materials for these
fibers.
The well-known embrittlement problem with SiC/C/SiC
composites in the intermediate temperature range (700
800C) has been analyzed in detail [1921]. An approach
borrowed from C/C composite technology has been applied
to this class of composites. Adding boron to the matrix
results in B2O3 formation in matrix cracks during exposure
at elevated temperatures, thereby sealing the cracks and
inhibiting oxidation of the pyrolytic carbon interface. The
key questions are can the oxidation occur fast enough at

Fig. 12. Thermal activation plots for average strength of as-produced Al2O3-based fibers at a gauge length of 25 mm [14].

R.E. Tressler / Composites: Part A 30 (1999) 429437

intermediate temperatures to prevent gasification of the C as


CO or CO2 and is the borosilicate glass impervious enough
to O2 at elevated temperatures to yield usable lifetimes in
composites with matrix cracks?
The use of BN coatings as a substitute for pyrolytic
carbon has been and is being researched rather intensely.
Chemical vapor deposition of the BN has become the
process of choice, and the microstructure and properties of
the resultant coating depend dramatically on the conditions
of deposition. Coatings of BN deposited at low temperatures
are amorphous or turbostratic while those deposited at high
temperatures (above 1500C) are hexagonal BN. Impurities of carbon and oxygen are common, particularly in BN
deposited at low temperatures. Recently, Si-doped BN has
been deposited on SiC fibers and shows considerable
promise as an oxidation resistant coating which retains
desirable mechanical properties.
The major issue with BN coatings is again the intermediate temperature oxidation and gasification of the oxide, in
this case as hydrated borate species. Our recent work on
SiC/BN/SiC composites has demonstrated that even the
pyrolytic BN deposited at 1800C is oxidized and volatilized in nominal 1 and 10% PH2 O ambients at 700 and
800C [22]. Other BN interphases testedCVD-BN
deposited at 1060 and 1400Cwere more severely
attacked under these conditions. However, a CVD-BN
doped with 22 wt% silicon deposited at 1400C showed
no volatilization of the interphase region under the above
conditions for times up to 1000 h. Clearly, more extensive
studies of the durability of this composite system are
warranted.
The recent work of Sun, Nutt and Brennan on a
Nicalon fiber reinforced glassceramic composite
which used a layered BN/SiC fiber coating indicates
that the matrix cracks can be effectively sealed by
this approach [23]. The compelling result is that a
sample statically stressed at 138 MPa (well above the matrix
cracking stress of 88 MPa) at 1100C in air lasted for over
1.7 years and the residual strength was similar to an
unoxidized sample.
Layered coatings such as BN/C/BN, BN/C/Si3N4, SiC/C/
SiC and BN/SiC and multilayers of these repeat units have
been evaluated in composites with SiC-based fibers. The
available data is rather sketchy as to whether or not the
oxidation problem in these nonoxide composites has been
measurably improved.
Luthra, on the basis of a kinetic model for oxygen diffusion through SiO2 which has the lowest oxygen permeability
of any oxide, has postulated that the oxidation protection of
a 1 mm coating of a silica forming material such as SiC is
limited to 100 h at 1200C in the presence of oxygen.
Therefore, he argues that a systems approach must be
taken to the oxidation resistance of the overall composite
which includes better coatings for fibers and techniques for
rapidly sealing cracks [24].
The prospect of in-situ coatings as in the SiBNC fiber

435

developed by Bayer is also an attractive approach to the


interphase problem, particularly in view of the high cost
of CVD or CVI coatings. Nitridation of B-containing
SiC fibers is an approach that is worth exploring more
extensively.
Oxide fiber reinforced oxide matrix composites are being
more actively pursued as our understanding of the limitations of the nonoxide composites is becoming more
complete, and as more creep resistant oxide fibers are
being developed. However, an effective coating for oxide
fibers that results in a crack deflecting interface remains to
be demonstrated in detail. Promising directions for such
interphases are briefly summarized here.
Porous coatings and porous matrices (without an interphase) have been prepared for oxide/oxide composites [25
27]. However, densification, pore coarsening and permeability to environmental degradants are all concerns for
long-lived composites at elevated temperature.
Fugitive interfaces have been pursued by several
researchers [2630]. Carbon coated fibers have been the
major focus of this work. In Nextel 720, fiber reinforced
calcium aluminosilicate glassceramic in which the carbon
coating had been removed, good strength retention was
demonstrated after a 500 h, 1000C unstressed heat treatment in air. The long term, higher temperature use of such a
concept seems suspect in view of the expected reactions
between the fiber and the matrix.
The more promising interfaces fall into the classes of
layered oxides (the oxide analog to C or BN) and nonwetting oxides (with alumina fibers, primarily). In the former
category, materials with both the b -alumina and the
magnetoplumbite structures have been studied. The mobility and volatility of alkali ions, particularly Na and K ,
in the b -alumina structure have frustrated attempts to use
these coatings with alumina fibers.
The magnetoplumbites, typified by hibonite, CaAl12O19,
contain alkaline earth ions which are less likely to migrate
and degrade the oxide fibers. Promising results have been
achieved with hibonite coatings on sapphire fibers [31, 32].
Technical challenges remain to incorporate this material
into a composite system where the fibers are polycrystalline
and of small diameter.
A class of layered perovskites has recently been investigated for interphase materials in oxides and composites
[33]. The compounds KCa2Nb3O10 and BaNd2Ti3O10 appear
to be stable with alumina to at least 1250C [34]. This work
is at an early stage.
The oxide compounds which have a high interface
energy with candidate oxide fibers or the matrix are
being researched actively in several groups [3537]. The
rare earth phosphates of the monazite family (larger ions)
and the xenotime family (smaller ions) are being studied.
In model system studies LaPO4 has been shown to debond
easily from alumina. However, it appears that achieving
precise stoichiometry is important to avoid degrading the
fiber. This compound also appears to be stable in contact

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R.E. Tressler / Composites: Part A 30 (1999) 429437

with Nextel 720, which contains SiO2 in the form of


mullite.
Other compounds of the general ABO4 stoichiometry are
also being researched; especially CaWO4 which has a high
melting point. Very promising results with CaWO4 and
ErTaO4 interphases on Nextel 610 fibers in composite
matrices of aluminaCaWO4 and aluminaErTaO4 have
been achieved by Goettler and co-workers with room
temperature strengths in undirectional composites of over
50 ksi and extensive fiber pullout [38]. The scheelite coating
also appears to behave similarly to the Nextel 720 fiber.
Clearly, considerable effort is warranted in this promising
area.
Progress in applying these coatings in a cost effective
manner is being made, primarily using solutions and slurries. Additional work is required to develop multiple
sources of coated fibers and fabrics.

[3]

[4]
[5]
[6]
[7]
[8]
[9]

[10]

[11]

3. Summary
Significant progress is being made in the development of
creep resistant fibers and crack deflecting, durable interphases for ceramic matrix composites. Silicon-carbidebased fibers, spun in the form of polymer precursors, with
near stoichiometric composition and low oxygen content are
exhibiting useful creep and rupture resistance to nearly
1300C (depending on the applied stress). A new amorphous
SiBNC fiber is reported to have better properties than
the crystalline fibers, plus it has the possibility of developing
an in-situ BN interphase. Although the recently introduced
aluminamullite composite oxide fiber is much improved in
creep resistance compared to earlier polycrystalline alumina
fibers, its properties are not adequate for applications above
1100C (using similar criterion as used for the nonoxide
fibers). Promising research directions for oxidation and
volatilization resistant interphases with the appropriate
mechanical properties for nonoxide composites are being
pursued. Silicon-doped BN interphases are much more
durable than BN, and multilayer interphases of C and SiC
and BN and SiC are also showing promise.
For the oxides, oxide coatings with layered crystal structures have shown some promise, but nonwetting oxides of
the monazite family (phosphates) and the scheelite family
appear most promising in recent studies. However, the
demonstration of a long lived oxide composite system
with a stable interphase for high temperature use is still an
unachieved goal.

[12]

[13]

[14]
[15]

[16]

[17]
[18]

[19]

[20]

[21]

[22]

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