Corhon. 197s. Vol. 13. pp.

159-166 Pergamon Pren Prmted in Great Brain

THE CHEMICAL VAPOR DEPOSITION

OF CARBON ON CARBON FIBERS*

H. 0. PIERSON and M. L. LIEBERMAN

SandiaLaboratorie5,AIbuquerque,NM871 I.U.S.A.

(&mired 12 July 1974)

Abstract-The relations between chemical vapor deposition (CVD) parameters and the resultant pyrolytic carbon
microstructures have been examined for matrix deposition in fibrous carbon substrates. The parameters considered
are temperature (1200-145O”C), pressure (20-630 Torr), C/H ratio (l/4-1/14), total flow rate (2-16) limin). and carbon
felt density (0.12-0.23 g/cm”). Most of the data obtained are in agreement with a CVD model for carbon; where
agreement is not obtained, it is surmised that the assumptions of the model may not be satisfied.

1. INTRODUCTION pressure, source gas C/H ratio, gas flow ral.e, and
Carbon-carbon composites, composed of fibrous car- substrate bulk density. While the last parameter is not
bon substrates and pyrolytic carbon matrices, have been strictly a CVD variable, it has been included because
shown to be suitable heat-shield materials because of their earlier work@] had shown that it also affects matrix
high thermal stress resistance [ 11. Both components microstructure. In all cases, carbon felts were used as
contribute to the resultant physical properties. The fiber deposition substrates. These were prepared by carboniza-
precursor and volume fraction are important substrate tion of polyacrylonitrile (PAN) fiber felts, as described
parameters[2-51. Similarly, the matrix microstructure has elsewhere [3]. All deposition conditions are given in Table
a significant effect on properties [f&9]. 1. Many of the experiments were repeated at least twice,
When the composites are examined under polarized particularly near critical conditions where a small change
light illumination, three major types of microstructure are
frequently observed[2, 6-8, 10-121. As shown in Fig. 1,
each type has unique optical characteristics. The smooth
laminar (SL) material exhibits large well-defined extinc-
tion crosses and few discernible growth features. In SMOOTHLAMINARISL)
contrast, the rough laminar (RL) matrix displays numer-
ous, irregular extinction crosses, many growth features,
and high optical reflectivity. The isotropic (ISO) deposit
exhibits few, if any, extinction crosses and has low optical
reflectivity.
Lieberman has established a chemical vapor deposition
(CVD) model for carbon which relates the gas phase
conditions to the resultant optical microstructure of the ROUGHLAMINARIRLI
deposit [lo, 131.Previous work has shown good agreement
between predictions of the model and experimental
results [8, 10, 11, 14, 151.The present study is an extension
of that work which has been expanded to include all of the
controllable deposition parameters. Its goal is to further
compare the predictions of the model with experimental
results so that relations between deposition parameters
and microstructure can be established.

2. EXPERIMENTAL
PROCEDURES
Eight sets of experiments were performed to examine
the CVD variables of mandrel temperature, total gas

*This work was supported by the U.S. Atomic Energy Fig. 1. Optical photomicrographs of carbon composites showing
Commission. three types of matrices. Polarized light illumination.

159
160 H. 0. PIERSON
and M. L. LIEBERMAN

Table 1. Chemical vapor deposition parameters of the various deposition experiments

CH, H* Ar
Experi- Bulk
mental Susceptor Partial Partial Partial density
Series temperature Flow pressure Flow pressure Flow pressure C/H felt
no. “C l/min Torr l/min Torr l/min Torr ratio g/cm’

1 1200”-1450” 2 630* 0 0 0 0 l/4 0.2

(25”increments)

2 1200”-1450” 2 315 2 315 0 0 l/6 0.2

(25”increments)

1275” 2 630 0 0 0 0 l/4 0.2

1275” 2 315 2 315 0 0 l/6 0.2
1275” 2 210 4 420 0 0 l/8 0.2
1275 2 158 6 472 0 0 l/10 0.2
1275” 2 105 10 525 0 0 l/14 0.2

1200”-1325” 2 100 0 0 0 0 l/4 0.2

(25”increments)

5 1125”-1325” 2 20 0 0 0 0 l/4 0.2

6 1275” 1 315 1 315 0 0 l/6 0.2

1275” 2 315 2 315 0 0 l/6 0.2
1275” 4 315 4 315 0 0 l/6 0.2
1275” 6 315 6 315 0 0 l/6 0.2
1275 8 315 8 315 0 0 l/6 0.2

7 1275” 2 630 0 0 0 0 l/4 0.2

1275 2 315 0 0 2 315 l/4 0.2
1275 2 210 0 0 4 420 l/4 0.2
1275” 2 158 0 0 6 472 l/4 0.2
1275 2 105 0 0 10 525 l/4 0.2

8 1275” 2 210 0 0 4 420 l/4 0.12

1275” 2 210 0 0 4 420 114 0.17
1275” 2 210 0 0 4 420 l/4 0.23

*630 Torr = local atmospheric pressure in Albuquerque, New Mexico.

in parameters resulted in appreciable microstructure
changes.
Infiltrations were performed by the thermal gradient
method [2,6] in which deposition initially occurs at the
heated mandrel-fibrous substrate interface. As deposition
proceeds, the pyrolytic carbon front moves out through
the thickness of the substrate. Methane was used as the
hydrocarbon source gas and the C/H ratio was varied by
means of hydrogen addition. Mandrel (susceptor) temper-
ature was monitored and controlled to ?lO”C. Total
pressure in the reaction chamber was maintained within
-+lO% at 20 and 1OOTorr; at local atmospheric pressure,
630 Torr, control was improved to about 1%. Each of the
gas flow rates was controlled to ~10%. The felt substrate
had nominal dimensions of 1.5 x 5 x 10cm.
After infiltration, specimens were removed from the
plates (Fig. 2) for standard metallographic exam-
ination[2]. Figure 3 presents a photomicrograph, taken
under polarized light, of a typical composite. It shows the
matrix sheath formed around each fiber and the intersec-
tions of several sheaths. The distribution of matrix
microstructures within a sheath is illustrated schemati-
cally in the same figure. The arrow AB represents a cross
section of the matrix, point A being the beginning of the
deposition and point B, the end. In this particular
example, the microstructure is SL during the first part of
deposition and RL during the remainder of the time.
Figure 4 contains four photomicrographs of cross
sections at different locations through the thickness of a
single composite. The diagrams to the right of the
photomicrographs are schematic representations of the
composite at each of the four points from the beginning
(point A) to the end (point B) of deposition. In this
particular example, the microstructure of the matrix in
photo No. 1 (inside) is entirely RL; the matrix in photo
No. 2 shows a band of SL around the fiber; in photograph
 The chemical vapor deposition of carbon on carbonfibers 161

BEGINNING OF DEPOSITION

i:?IS FACE
rOLlSiiE0

i i \ d.SiDE
(WSCEPTORSIDE)
FYBERMATRIX INTERFACE
Fig. 2. Method of preparing sample for metallography.
Fig. 3. Optical appearance of matrix microstructure as it is
No. 3 this SL band is larger and finally in photo No. 4 the deposited around a fiber.
microstructure is entirely SL.
These four photomicrographs are illustrative of the above. The steps are summarized in the bar diagram at the
microstructure distribution analysis carried out from the far right in Fig. 4. This graphic illustration is used later to
inside to the outside of each composite plate as mentioned describe the experimental results.

\ INSIDEWSCEPTORSIDE)
cm!
SL RL

BEGINNINGOF DEPOSITION\ ENDOF

(FIBER-MATRIX INTERFACE) EPOSITION

'OUTSIDE
/

UTSIDE 6
/

Fig. 4. Photomicrographs and graphic illustration of matrix microstructure at various points through the thickness of
a plate.
162 H. 0. PIERSON
and M. L. LIEBERMAN
3. RESULTSANDDISCUSSION
3.1 General trends
During the course of the present investigation, some
microstructure trends were observed which can be
summarized in the following generalized statements:
I. The boundary between an SL and RL matrix is sharp
and well defined without any noticeable transition zone.
2. The boundary between RL and IS0 is diffuse and
poorly defined with a transition zone in which the RL
matrix shows a grain structure that becomes smaller and
smaller as it gradually merges into the IS0 structure.
3. The optical reflectivity of SL microstructures under
polarized light varies from high (close to RL) to very low
(similar to ISO). This is in agreement with other work [111.
4. IS0 microstructures show little optical reflectivity
and at times exhibit well defined extinction crosses. Thus,
it is often difficult to distinguish SL from IS0 microstruc-
tures particularly for matrices deposited at low pressure.
5. The matrix deposited around the fiber may be all of
one type, SL, RL or IS0 as in Fig. 1. Or, as is very often
the case, it may be a combination or banded matrix
starting for instance by SL followed by RL as in the
examples of Figs. 3 and 4. Whenever a banded matrix
occurs, a SL microstructure is never directly followed by
an IS0 (or vice versa) but always by an RL. The sequence
of events is always SL to RL to IS0 (and vice versa).
3.2 Comparison of observed and predicted microstruc-
tares-basis of comparison
The CVD model developed by Lieberman[lO] relates
microstructure to the gas phase concentrations of
acetylene, CzH2, and benzene, C6H6. As the gas phase
molar ratio R = CzHz/CsHnincreases, microstructures are
predicted to occur, under non-sooting conditions, in the
order SL + RL + ISO. Equilibrium values of R have been
calculated previously[13] and are found to generally
FIBERMATRIX INTEFACE
IBEGINNINGOFDE~OSITIONI ,ENDOF DEPOSITION
DEPOSlTlONTEMPERATURE,'C
Fig. 5. Microstructure of carbon matrix as a function of deposition temperature at 630Torr and C/H = l/4
(experiment No. 1).
increase with increasing temperature, decreasing pres-
sure, and decreasing C/H ratio[8,13]. The model is based
on a series of assumptions, one of which is the existence
of gas phase equilibrium at or near the deposition surface.
As will be discussed later, this assumption may represent
a limitation on the applicability of the model.
For the deposition experiments performed in this study,
the observed initial microstructures (Figs. 5-12) and
calculated equilibrium values of R are given in Tables 2-7.
The initial microstructure is defined as the microstructure
of the deposit nearest to the susceptor and first around the
fiber. There the CVD parameters are relatively well
defined, since the deposition temperature is essentially
that of the mandrel and the C/H ratio has not yet been
changed by hydrogen accumulation resulting from
pyrolysis reactions[8]. This allows a comparison of the
experimental results with predictions of the model.
3.3 E$ect of temperature
It was originally thought that the temperature of
deposition was the major factor controlling microstruc-
ture. This led to the assumption that the differences
between the two methods of CVD infiltration, the
“thermal gradient” and the “isothermal” were due to
differences in temperature[l2, 161. It now appears that
temperature, although important, is no more critical than
the other CVD parameters such as pressure and C/H
ratio.
Figure 5 shows the relationship between temperature
and microstructure at a C/H ratio of l/4 (100% methane).
The initial microstructure is SL below 1300”, RL from
1300°C to 1375°C and IS0 above 14Oo”C,(Table 2).
Figure 6 shows the same relationship as Fig. 5 but with
a C/H ratio of l/6 (with hydrogen dilution). Again below
13OO”C,the initial microstructure is SL, from 1300°C to
1325°CRL and above 1350°CIS0 (Table 3). In both cases
(Figs. 5 and 6), increasing the temperature changes the
 The chemical vapor deposition of carbon on carbon fibers 163

FI3ERhlATRlXINTERFACE
IREGINNINGOF DEPOSITION) ENDOF DEPOSITION

I225 1250 I275 1300 1325 1350 1375 I400 1425

DEPOSlTIO"d
TEhlPERATURE C

Fig. 6. Microstructureof carbon matrix as a function of deposition temperature at 630Torr and C/H = l/6
(experiment No. 2).

Table 2. Effect of temperature on equilibrium C,H,/C,H, initial microstructure from SL to RL to ISO. These figures
ratio (R) and relation with initial microstructure with C/H ratio also show that it is impossible to obtain an all RL
of l/4
microstructure within these conditions.
Observed
Calculated initial 3.4 Effect of C/H ratio
Temperature C,H,/C,H, ratio microstructure Figure 7 shows the effect of varying the C/H ratio (that
“C (R) (Fig. 5) is the C/H ratio of the CR/R mixture entering the
1200 0.8 SL reaction chamber), while maintaining the susceptor
1225 - SL temperature at 1275°C and the total pressure at 630 Torr
1250 1.6 SL (local atmospheric pressure in Albuquerque, N. M.). The
1275 - SL initial microstructure is SL up to C/H = l/8, RL for
1300 3.3 RL
1325 - RL
C/H= l/IO and IS0 at C/H= l/14 (Table 4). Thus
1350 7.1 RL decreasing the C/H ratio leads to an IS0 microstructure
1375 - RL and has the same effect as increasing temperature
1400 17.0 RL (corresponding to an increase in R).
1425 IS0 So far, in both variables, temperature and C/H ratio,
1450 45 IS0
only the initial microstructure has been considered. Let us
Note: Pressure = 630 Torr. now analyze the microstructure at another point along the
thickness of the felt and later during the deposition, In
Figs. 5 and 6, as deposition proceeds, the microstructure
Table 3. Effect of temperature on equilibrium C,H,/C,H, changes from SL to RL to IS0 (particularly in the inside
ratio (R) and relation with initial microstructure with C/H ratio
of l/6

Observed
Calculated initial FIBERMATRIXINTERFACE
IBEGINNINGOF DEPOSITIONI END OF DEPOSITlOh
Temperature C,H,/C,H, ratio microstructure /
“C (R) (Fig. 6)
INSIDE
1200 1.3 SL ISUSCEPTORSIDE)
1225 - SL
1250 2.6 SL
1275 - SL
1300 5.7 SL
1325 - RL OUTSIDE\
1350 12.8 RL
1375 RL I!4 Ii6 II8 l/IO Ill4
1400 31 IS0 C'H RATIO
1425 - IS0
Fig. 7. Microstructure of carbon matrix as a function of C/H ratio
Note: Pressure = 630 Torr. at 630Torr and 1275°Cdeposition temperature (experiment No. 3).
164 H. 0. PIERSON
and M. L. LIERBERMAN

Table 4. Effect of C/H ratio on equilibrium CzH2/CaH6 0% @$jR,

ratio (R) and relation with initial microstructure at 127s”
FIBER MATRIX 1NlERFACE
and 630Torr
IBEGINNIECOF DEPOSITION) ,END OF DEPOSITION

Observed
Calculated initial
C,H,/C& ratio microstructure
C/H ratio (R) (Fig. 7)

114 2.3 SL
l/6 3.8 SL
l/8 6.0 SL
l/IO 8.4 RL
l/14 20.5* IS0

*Extrapolated value. Fig. 8. Microstructure of carbon matrix as a function of deposition

temperature at 100Torr and C/H = l/4 (experiment No. 4).

half section of the felt, next to the susceptor). According

to the CVD model, this indicates either a rise in
temperature, which is not possible since the initial
FIBER-MATRIXINTERFACE
microstructure is already at susceptor temperature, or a
IBEGINNINGOF DEPOSlTlONl ENDOF DEPOSITION
decrease in the C/H ratio. It has been previously \ /

postulated[8] that, as the plates densify and the porosity

INSIDE t
decreases, the effective residence time of the gas is WJSCEPTOR SIDE) z
increased. This in turn permits additional gas phase x
2
reaction which produces more gas molecules than are E
entering the reaction zone. As a result there is a hydrogen 2
2
concentration gradient with the highest concentration of
OUTSIDE
hydrogen (or lowest C/H ratio) occurring toward the end
_-L
of the densification (right side of the bars). Thus the 1125 1175 1225 1275 1325
changes in the microstructures from the inside to the
DEPOSITIONTEMPERATURE."C
outside of the plate and from the start to the end of the
deposition may be related to changes in C/H ratio. Fig. 9. Microstructure of carbon matrix as a function of deposition
Dilution with hydrogen (decreasing the C/H ratio) has a temperature at 20Torr and C/H = l/4 (experiment No. 5).
beneficial aspect which is not reflected in the model. That
is, the microstructure is less sensitive to experimental
Table 5. Effect of temperature on equilibrium C2H2/C&
variations Figure 5 (no hydrogen dilution) is actually the ratio (R) and relation with initial microstructure at C/H = l/4
result of several infiltrations at each temperature and what and 100Torr
is shown is an average representation of the microstruc-
ture. In many cases, the results would overlap in the Observed initial
microstructure
adjoining temperature bracket. On the contrary, in the set Calculated (non-equilibrium
of experiments of Fig. 6 (C/H = l/6) the results were more Temperature C2HJCsHs ratio conditions)
consistent and fewer experiments were needed to “C (R) (Fig. 8)
establish a trend.
1200 4.5 SL
1225 SL
3.5 E$ects ofpressureand $0~ rate 1250 12.5 SL
1275 SL
Figures 8 and 9 show the effect of varying temperature
1300 38 SL
at two reduced pressure levels, 100 and 20 Torr. Tables 5 1325 128 SL
and 6 show that the observed initial microstructures no
longer correspond to the boundaries of R determined in
the other experiments. One can surmise that the CVD This implies that the system is further removed from
model does not apply here because the assumption of gas equilibrium. Other work[l5] has shown that the reduced
phase equilibrium is no longer valid. At the reduced effective residence time of the gas in the heated zone
pressures considered in this study (100 and 20 Torr), the leads to a reduced extent of gas phase reaction.
linear gas velocities are 6.3 and 31.5 times higher Increasing the flow rate also yields a general shift
(respectively) than that at local atmospheric pressure [ 171. toward the low R microstructures RL and SL (Fig. 10).
 The chemical vapor deposition of carbon on carbon fibers I65

Table 6. Effect of temperature on equilibrium C2H2/C6H6 ratio (R\

and relation with initial microstructure at C/H = l/4 and 20 Torr
FIYFR ClATRlX lYKRfhCE
'?E',IlUNS OF DEPOSlTiONi END OF DEPOSITION
Observed /

microstructure
Calculated (non-equilibrium
Temperature C2H&H, ratio conditions)
“C (R) (Fig. 9)

1125 5.5 SL
1175 20 SL
1225 73 IS0
1275 320 IS0
1325 1400 IS0

?EIHANL PARTlA "RESII!RI TORR

Fig. 11. Microstructure of carbon matrix as a function of partial

pressure of methane with argon diluent, C/H = l/4. 1275°C
deposition temperature (experiment No. 7).

Table 7. Effect of partial pressure of methane on equilibrium

CZH,/ChH6 ratio and relation with initial micro@ructure at
C/H = l/4 and 1275

Partial Pressure Calculated Observed

Torr C,H&H, ratio microstructure
CH, Argon (R) (Fig. II)

630 0 2.3 SL
315 315 5.3* SL
210 420 9,0* RL
157 473 13* RL
105 525 20 IS0
Fig. IO. Microstructure of carbon matrix as a function of flow rate
at 630Torr, C/H = l/6, and 1275°C deposition temperature *Extrapolated values.
(experiment No. 6).

is entirely RL. Repeated experiments show this to be

This implies that as the flow rate increases the system reproducible. The reason for this is shown in Table 8
becomes further removed from the gas phase equilibrium which gives the value of R at 1250, 1275 and 1300°Cat a
condition. C/H ratio of l/4 as well as those for C/H ratios of l/4 and
l/5 at 1275°C. It can be seen that at 157Torr partial
3.6 Effect of argon dilution pressure of methane the values of R all fall within the
Figure 11 shows the relationship between partial range of 8.3 to 20 which is the range of RL formation.
pressure of methane (diluted with argon to 630 Torr) and Therefore neither a change of temperature of 25°C nor a
the microstructure at 1275°C. Since no hydrogen is used
the C/H ratio is l/4. Partial pressures of methane are 630, Table 8. Variations of the calculated equilibrium C2HJChH, ratio
315, 210, 157 and 105 Torr. (R) with partial pressure of methane over a range of temperature
Table 7 shows that the initial microstructure is SL to a and C/H ratio
value of R of 5.3, RL from approximately 7 to 18 Calculated R at
(extrapolated values) and IS0 at 20 and above. Again the
predictions of the model are verified. Thus, lowering the Partial C/H = l/4 1275°C
pressure of
partial pressure has the same effect as increasing the
CH, (Torr) 1250” 1275” 1300 C/H = 114 C/H = I/5
temperature or decreasing the C/H ratio (in all cases this
means an increase in R)[14]. 630 1.5 2.3 3.0 2.3 2.9
When argon dilution is used, the microstructure 315* 3.7 5.3 8.3 5.3 6.4
throughout the felt is considerably more uniform than 210* 5.5 9.0 14 9 IO
157* 8.3 I3 20 I3 I5
when one uses undiluted methane at 630Torr (Fig. 5) or 105 13 20 36 20 24
methane diluted with hydrogen (Fig. 6). For instance, at
157 Torr partial pressure of methane, the microstructure *Extrapolated values
166 H. 0. PIERSONand
change in C/H ratio from l/4 to l/5 (which might result
from changes in local conditions within the thickness of
the felt) would affect the microstructure; it would remain
RL. At 630 Torr and 3 15Torr the range covers R values
that would result in both RL and SL microstructures and
at 105 Torr both RL And IS0 microstructures. These
conclusions are in agreement with the experimental
results (Fig. 11).
/--Jt qjRI
FIBER-MATRIX INTERFACE
BEGINNINGOFDEPOSlTlO~ ENDOF DEPOSITION
/ lower and higher values, respectively. In terms of CVD
BULK DENSITYOFFELT SUBSTRATE,G/CM'
Fig. 12. Microstructure of carbon matrix as a function of bulk
density of felt at 630Torr total pressure (157Torr partial pressure
of methane with argon diluent), 1275°Cdeposition temperature,
and C/H = l/4 (experiment No. 8).
3.7 E#ect of felt bulk density
Fig. 12 shows the effect of the bulk density of the felt on
the microstructure using partial pressure of methane (157
Torr methane, 473 Torr argon) at 1275°C. At a bulk
density of 0.23 g/cm’ no SL is noted but at 0.17 g/cm’ a
small amount of initial SL is noted toward the inside
(susceptor side) of the felt, at 0.12 g/cm’ the amount of SL
is considerably greater. This confirms the findings of Ref.
8. One may assume here that the lower density felt is
closer to the model since an increase in the fiber volume
has the effect of increasing the effective residence time of
the gas in the hot zone. Under the deposition conditions of
the experiment SL is probably the model prediction. But
as density increases, hydrogen concentration increases
and the initial deposit shifts from SL to RL. Therefore
increasing the bulk density of the felt has the same effect
as increasing temperature or decreasing the C/H ratio.
4. CONCLUSION
These experiment9 on the CVD of carbon from
methane confirm previously reported work[4, 8, 11, 141
and show that the predictions of the model for deposition
of carbon apply to deposition on fibrous carbon sub-
strates, within the following limitations:
a. Only when the initial deposit is considered (where
the deposition parameters are known accurately), can a
correct microstructure be predicted.
M. L. LIEBERMAN
b. The sensitivity of microstructure to flow rate implies
that the model will not give accurate predictions in cases
where the assumption of gas phase equilibrium is not
valid.
Based on the large quantity of experimental data now
available, it appears possible to establish a set of
guidelines relating the CVD parameters to the result-
ant microstructures.
1. The sequence SL-RL-IS0 is generally observed.
2. Phase boundaries are related to the C2H&,Hs (R)
ratio; RL forms when R = 5-20, while SL and IS0 form at
parameters this means the order SL-+RL-+ISO is
obtained for increasing temperature, decreasing C/H
ratio, decreasing pressure, and increasing substrate fiber
volume.
Acknowledgements-The authors wish to thank B. Granoff for his
valuable technical assistance in the area of microstructure
characterization, R. M. Curlee for his advice regarding deposition
conditions with argon dilution, and .I. F. Smatana for technical
assistance in the experimental work.
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