Ada 306408

NASA CONTRACTOR NASA CR-809
REPORT
Os
09
19960405 024
THERMOPHYSICAL PROPERTIES OF
A LOW-DENSITY PHENOLIC-NYLON
ABLATION MATERIAL
V
by W. T. Engelke, C. M. Pyron, Jr., and C. D. Pears
Prepared hy
SOUTHERN RESEARCH INSTITUTE
Birmingham, Ala.
for Langley Research Center
NATIONAL AERONAUTICS AND SPACE ADMINISTRATION WASHINGTON, D. C. JULY 196
04
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THIS DOCUMENT IS BEST
QUALITY AVAILABLE. THE
COPY FURNISHED TO DTIC
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NOT REPRODUCE LEGIBLY.
NASA CR-809
THERMOPHYSICAL PROPERTIES OF A LOW-DENSITY
PHENOLIC-NYLON ABLATION MATERIAL
By W. T. Engelke, C. M. Pyron, Jr.,

and CD. Pears
Distribution of this report is provided in the interest of

information exchange. Responsibility for the contents
resides in the author or organization that prepared it.
Prepared under Contract No. NAS 1-2978 by

SOUTHERN RESEARCH INSTITUTE
Birmingham, Ala.
for Langley Research Center
NATIONAL AERONAUTICS AND SPACE ADMINISTRATION
For sale by the Clearinghouse for Federal Scientific and Technical Information
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î-'-'ii-t'.i'X'i''" IM. ~^":~'ri:p~Tr

THERMOPHYSICAL PROPERTIES OF A
LOW-DENSITY PHENOLIC-NYLON ABLATION MATERIAL
By W. T. Engelke,
C. M. Pyron, Jr. , and C. D. Pears
Southern Research Institute
SUMMARY
Some physical properties were determined on a low-density phenolic-

nylon that was both nondegraded (virgin) and thermally degraded (charred).
The work was performed under Task Order 4 of Contract NAS 1-2978,
which was a continuation of similar studies under previous Task Orders 1
through 3. Task Orders 1 through 3 have been reported in NASA TN D-2991
(Reference 1).
The low-density phenolic-nylon was a molded composite consisting

of 25% phenolic resin, 35% phenolic Microballoons, and 40% powdered nylon.
The material was thermally charred in an arc tunnel.
The thermal conductivity of the virgin material from -200°F to 750°F

ranged from 1. 27 x 10-5 Btu/sec/ft/°F (7. 91 x 10"2 W/m/°K) to a maximum
of 1. 69 x 10"5 Btu/sec/ft/°F (10. 5 x 10-2 W/m/°K). These values were
lower than those exhibited for the low-density phenolic-nylon evaluated
under Task Order 1. The reason for the lower conductivity appears to be
the weaker structure of the material evaluated under this program.
The thermal conductivity from 1000°F to 5000°F of the charred material

increased from 11. 5 x 10"5 Btu/sec/ft/°F (0. 72 W/m/°K) to 76 x 10-5 Btu/
sec/ft/°F (4. 73 W/m/°K). During cooling the values were higher and more
scattered, indicating further degradation at the higher temperatures and
some shrinking and cracking of the specimens upon cooling.
The heat capacity of the virgin material increased from 0. 20 Btu/lb/°F

(837 J/kg/°K) at -200°F to 0. 58 Btu/lb/°F (2427 J/kg/°K) at 600°F. Due to
the carbonaceous character of the charred material, the heat capacity
compared well with that of graphite. The values increased from 0. 39 Btu/lb/
°F (1632 J/kg/°K) at 1000°F to 0. 57 Btu/lb/°F (2385 J/kg/°K) at 5000°F.
The coefficient of thermal expansion at 70°F for the virgin material
was 23.5 x 10"6 in./in./°F (42.3 x 10"6 m/m/'K). The data indicated slight
anisotropy of the material and also demonstrated a transformation of the
material above 230°F which caused the material to contract.
The permeability of both the virgin and charred material was obtained
at low pressure drops across the specimen with helium and nitrogen used as
the permeating gases. The admittance oi the Virgin specimens ranged from
3. 6 x 10"4 m2/sec to 5. 2 x 10"4 m2/sec, and the charred material exhibited
values from 0.81 m2/sec to 1.87 m2/sec. The flow through the charred
specimen was transitional and turbulent.
The total normal emittance of the char from 1500°F to 5000°F ranged
from 0.79 to 0.87.
The mechanical properties of the virgin material from -200°F to 750°F

were determined. The ultimate tensile strength decreased from 570 psi
(3. 93 x 106 N/m2) at -200°F to below 100 psi (0. 69 x 106 N/m2) at 500°F.
The ultimate compressive strength decreased from 2600 psi (17. 03 x 106
N/m2) at -200°F to approximately 200 psi (1. 38 x 10* N/m2) at 750°F. Both
tensile and ultimate strength values were lower (about one-half) than those
of the phenolic-nylon evaluated under Task Order 1. The weaker structure,
mentioned before, was apparently the reason for the lower values.
INTRODUCTION
This is the final report on the thermophysical property evaluation of

a low-density phenolic-nylon ablation material performed for the NASA
Langley Research Center under Contract No. NAS 1-2978, Task Order 4.
The physical properties of the low-density phenolic-nylon in both the non-
degraded (virgin) and thermally degraded (charred) forms were determined
and analyzed. This investigation was performed to characterize the material
for its reentry application as an ablative heat shield. The program was a
continuation of similar studies performed under the previous Task Orders 1
through 3 reported in NASA TN D-2991 (Reference 1).
Specifically, the thermal conductivity, heat capacity, thermal expansion,

density, permeability, and mechanical properties were determined on the
virgin material; and the thermal conductivity, heat capacity, total normal
emittance, density, porosity, and permeability were determined on the charred
material. The temperature ranges were -200°F to 750°F for the evaluation
of the virgin material and 1000°F to 5000°F for the charred material.
Reference 1 briefly describes the apparatuses and summarizes the
measurement procedures that were applied, except for the permeability
measurements. Additional details concerning the test methods may be
found in references cited in the discussion of data.
SPECIMEN MATERIAL
The low-density phenolic-nylon material was supplied by the NASA

Langley Research Center in both the nondegraded and thermally degraded
forms. The nondegraded material was supplied in a block 12 inches in
diameter and 4 inches thick. The thermally degraded material was supplied
in 3 inch diameter discs with the charred area approximately -j inch deep.
This low-density phenolic-nylon composite was molded and consisted

of the following materials: (1) 40%(weight) powdered 66 nylon, DuPont's
Zytel 103; (2) 25% (weight) phenolic resin, Union Carbide Corporation's
BRP-5549; (3) 35% (weight) phenolic Microballoons, Union Carbide
Corporation's BJO-0930. The molding was performed at a maximum
pressure of 2200 psi (15. 17 x 106 N/m2) and temperature of 340°F. The
material was also post cured at a maximum temperature of 300°F. The
complete molding and post curing history are shown in Figures 1 and 2.
A more thorough description of the individual constituents is included

in Appendix A. The difference in composition noted between this material
and the low density phenolic-nylon evaluated under Task Order 1 is the
different percentages of the constituents. The material under Task Order 1
contained 50% nylon, 25% resin and 25% Microballoons, and as discussed
later, was stronger and exhibited a higher thermal conductivity. Under a
separate contract study, reported in Reference 2, it was concluded that
the formulation and processing of the material under this present program
were less than optimum for a plastic composition. The formulation was low
in volume fraction of phenolic resin and the processing method caused
mechanical damage to the Microballoons and large temperature gradients
during processing. Thus as reported in subsequent sections, the lower
mechanical strength and thermal conductivity of this material when compared
to the material evaluated under Task Order 1, may be directly correlated with
the formulation and processing of the ablation material.
The thermally degraded material was produced in an arc tunnel. The
three inch diameter discs of the phenolic-nylon were exposed to the following
test conditions to form the chars: a stagnation enthalpy of 2800 Btu/lb (6. 5 x
106 J/kg), stagnation pressure of 0. 57 atm (5. 8 x 104 N/m2), thermal flux
at the material surface of 140 Btu/ft2/sec (1. 58 x 106 W/m2), freestream
Mach number of 3.0 with nitrogen gas and an exposure time of 90 seconds.
The arc tunnel is that described in NASA TN D-1621 with modifications to
provide for supersonic flow.
To further define the as received material, the densities of both the

virgin and charred materials were obtained. For the virgin material, the
bulk density was determined at room temperature by the water displacement
of a paraffin coated specimen in accordance with the ASTM D311-58 proce-
dure. The duplicate values obtained from two pieces selected at random
were 36. 8 lb/ft3 (589 kg/m3) and 36. 3 lb/ft3 (582 kg/m3) providing an average
density of 36. 6 lb/ft3 or 586 kg/m3. The density above and below room
temperature was adjusted with the thermal expansion data (reported under
the thermal expansion section) and is shown in Table 1. The density was
not calculated above 200°F since the thermal expansion data indicated a
transformation or initial degradation above this temperature which was
accompanied with some weight loss as indicated in the heat capacity data.
This, along with erratic expansion observed above 200°F, would make
calculations meaningless.
The bulk density of the char was also determined in accordance with
ASTM D311-58, and the true density was determined from a pulverized
sample by employing a pycnometer. The average bulk density, determined
from duplicate measurements, was 15 lb/ft3 (240 kg/m3), and the average
true density was 93. 6 lb/ft3 (1500 kg/m3). The volume percentage of
porosity, which is the ratio of the difference between the true and bulk
densities.over the true density, was 84% .
A micrographic evaluation was also performed on the char to deter-

mine the average pore size and relative frequency distribution. The two
specimens (^ in. thick) evaluated were taken from the top surface of the
char. The specimens were impregnated with polyalphamethylstyrene and
polished. The specimens were viewed at lOOX magnification in a plane
parallel to the thickness direction, and the pores were counted and measured
with a calibrated eye-piece. Figure 3 is a typical photomicrograph of the
char structure. The average pore diameter was 28. 8 microns, and the
histogram of pore diameters is shown in Figure 4. As can be seen in
Figure 3, the pore structure is rather irregular with wide variation in size.
In comparing this char with the previous degraded low-density phenolic-
nylon evaluated under Task Order 3, it was observed that the average pore
size was larger for this material; however, the density and porosity were
the same.
THERMAL CONDUCTIVITY
The thermal conductivity was determined in one direction (thickness

of the supplied block) on both the virgin and charred material. For the
virgin material, data were obtained from -200°F (144°K) to 750°F (673°K).
The temperature range for the charred material was from 1000°F (811 °K)
to 5000°F (3033°K) with the data being obtained during heating and cooling
cycles. The thermal conductivity of the virgin material was determined
using an ASTM C177 guarded hot plate apparatus. The char specimens
were evaluated in the radial inflow apparatus.
Apparatus and Procedure
ASTM guarded hot plate. - The 7-inch diameter ASTM C177 guarded
hot plate apparatus employed for the thermal conductivity evaluation of the
virgin material is described fully in Reference 3 and briefly below.
Basically this apparatus consisted of a central heater plate surrounded

by a guard heater, each separately controlled. The guard ring was main-
tained at the same temperature as the central heater so that all of the heat
flow was normal to the specimen surfaces. The heater plate was centrally
sandwiched between layers of filler material, hot face thermocouples, the
specimen, cold face thermocouples, filler material, a copper plate, and
finally a cold plate to dissipate the heat. In addition to the thermocouples
in contact with the specimen, thermocouples were located in the central
heater and the outer copper cold plates. Intimate contact was provided at
all interfaces by pressing the entire assembly together with a screw loaded
frame.
Filler pads of gum rubber were used from -200°F to 150°F. Above
150°F, Fiberfrax paper was used for the filler pads with a sheet of gum
rubber at the cold plate. Overlapping data were obtained at the 150°F
temperature level for both filler arrangements, providing a check on
contact resistance resulting from irregularities of the specimen surface.
To obtain mean temperatures of -200°F, liquid nitrogen was circulated
through the cold plate. For higher temperatures, chilled trichloroethylene
and water cooling were employed. When data points were obtained below
room temperature, the apparatus was enclosed in a plastic bag which was
purged with dry helium to eliminate frosting and moisture condensation.
During the run on Specimen 2, the change in thickness at the higher

temperature levels was monitored. This was accomplished by cutting slots
in the edge of the specimens. Small pads of 5 mil stainless steel shim stock
were placed above and below the specimen, and the distance between these
was measured with a hole gage. Measurements were taken at each tempera-
ture level. There was some uncertainty in these measurements since the
specimen degraded and collapsed more rapidly at the edge than at the center
due to the greater oxidation at the edge. This uncertainty was corrected at
the last point by measuring the thickness at the center of the specimen after
the completion of the run. The measurements taken at the intermediate
temperatures were corrected in proportion to the difference obtained on this
last point between the thickness change at the edge and at the center. The
uncertainties resulting from this procedure are recorded with the data. In
general, the thickness changed by about 20% during the run, and this change
could be measured within an uncertainty of 3% at temperatures below about
400°F and within 8% at higher temperatures where degradation of the material
was more severe.
Radial inflow apparatus. - To determine the thermal conductivity of

the char specimens a modified procedure of the radial inflow apparatus was
employed. The basic apparatus is fully described in Reference 1 and Refer-
ence 4.
Briefly, the test section was heated radiantly in a high temperature

furnace which employed a cylindrical graphite resistance heating element.
The heat flowed radially inward through the specimen to a central water
flow calorimeter. Water temperatures in the calorimeter were indicated
by thermocouples in the water stream located one-half inch apart, axially,
and heat flow through the specimen gage section was computed from mea-
surements of water flow rate and temperature rise. Specimen tempera-
tures were measured in two axially drilled holes located on two different
radii. Below 2000°F, temperature measurements were taken with chromel-
alumel thermocouples; above this temperature, measurements were taken
by sighting the bottom of the holes, by using an optical pyrometer and a
right angle mirror device. Axial conduction in the specimen is minimized
by (1) insulating the specimen on each end with graphite sleeves filled with
thermatomic carbon, (2) by making the specimen length at least twice the
gage length, and (3) by providing an isothermal hot zone over at least twice
the specimen length.
6
Thermal conductivity is calculated from the standard relation
k
= äAT U
where k is the thermal conductivity, A is the log mean cylindrical area, and
1 is the radial distance over which AT is measured.
To measure the thermal conductivity of the char specimens, the

technique described above was modified as follows: Four char strips,
approximately | inch wide by ^- inch thick by 2 inches long were arranged
symmetrically as shown in Figure 5. For this configuration, it was
necessary that isothermals in the specimen be perpendicular to the thick-
ness direction. This condition was achieved by placing thin strips of
pyrolytic graphite at the inner surfaces of the char strips. Because of
the high anisotropy of this material (the conductivity is approximately 50
times greater in the "a" direction than in the "c", or thickness, direction)
the isotherms were forced to assume a square configuration. Heat flow
other than through the specimen was eliminated essentially by using
thermatomic carbon of extremely low thermal conductivity (approximately
0.1 Btu/hr/ft2/°F/in.) as packing at the edges of the specimens. The space
around the calorimeter was packed with graphite. Temperatures were
measured at two locations in the strips, using the methods described
above. This procedure was employed with good results under previous
Task Orders 2 and 3, and is reported in NASA TN D-2991.1*
During each run, the thermal conductivity was determined while the
specimen was heated from 1000°F to 5000°F at 500°F intervals and cooled
from 5000°F to 1000°F at 1000°F intervals. This was done to determine
any alterations of the char after heating to the higher temperatures.
The machining of the conductivity specimens was performed after

impregnating the char with polyalphamethylstyrene to provide sufficient
mechanical strength. The evaluations were made after installing the
specimens in the apparatus and heat soaking them at 1000°F. At this
temperature, polyalphamethylstyrene effectively vaporized, leaving no
residue. This technique was also employed successfully under Task
Orders 2 and 3. The impregnation of the char was required only on the
thermal conductivity specimens and the photomicrographic samples.
*See REFERENCES
Data and Results
Virgin material. - The thermal conductivity data for the virgin

material are presented in Figure 6 and Table 2. As shown in the figure,
the conductivity increased sharply from 1. 27 x 10"5 Btu/sec/ft/°F (7. 9l'x
10-2 W/m/°K) at -250°F to 1. 69 x 10"5 Btu/sec/ft/°F (10. 52 x 10-2 W/m/
°K) at -100°F, then decreased to 1.27 x 10"5 Btu/sec/ft/°F (7.91 x 10"2 W/
m/°K) at 0°F. From 0°F to 750°F the values increased steadily to 1. 49 x
10" (7. 73 x 10" W/m/°K). These values were lower than those exhibited
by the phenolic-nylon material evaluated under Task Order 1; however, the
characters of the curves were very similar. The lower conductivity of this
material, which exhibited the same density as the previous phenolic-nylon,
may have resulted from weaker bonding (higher thermal contact resistance)
between the resin and filler. This obviously resulted from the formulation
and processing being less than optimum for a plastic composition as discussed
previously. As discussed in a subsequent section, the lower mechanical
properties exhibited by this material also indicate the weaker bonding.
Charred material. - The thermal conductivity values of the charred

material are shown in Figure 7 and Table 3. The conductivity and mean
temperature were computed by assuming a linear gradient through the
specimen as has been done in the past. As shown in the figure, the values
increase steadily from 11. 5 x 10~5 Btu/sec/ft/°F (0. 72 W/m/°K) at 800°F
to 76 x 10"5 Btu/sec/ft/°F (4. 73 W/m/°K) at 5000°F during the heating cycle
and during cooling the values decreased from 85. 6 x 10"5 Btu/sec/ft/°F at
4300°F to 34. 7 x 10"5 Btu/sec/ft/°F at 1500°F. It was found that the thermal
conductivity of the material during heating could be described by the equation,
k = 11.57 x 10_5 +5.3 x 10"15T3 (2)
where
k z thermal conductivity, Btu/sec/ft/°F
T = mean temperature of specimen, °F
Because of the scatter in the cooling data, these are not represented
by an equation but are shown as a band in Figure 7. During heating the
runs on three separate specimens agreed well; however, the cooling data
were scattered and higher than the conductivity during the heating cycle.
Examinations of the specimens after the run revealed that cracking and
shrinkage had occurred during cooling, and the structure appeared to be
more porous. These effects would tend to scatter the data and cause higher
indicated conductivities due to the increased radiant (and possibly convec-
tive) heat transport. The values obtained on cooling should be treated
with caution. Figure 8 illustrates the structural changes of the specimens
after exposures to 5000°F. Some erosion can be observed near the ends
of the strips, however, the central j inch gage lengths through which the
conductivity was measured appear to be undamaged.
HEAT CAPACITY
The enthalpy and heat capacity were determined on both the virgin
and charred material. The data were determined from -200°F to 750°F
for the virgin material and from 1000°F to 5000°F for the charred material.
Two apparatuses were used in the determinations. For the evalua-

tions of the virgin material, a drop type adiabatic calorimeter was employed.
A drop type ice calorimeter was utilized in the evaluations of the char material.
Adiabatic calorimeter. - This apparatus is fully described in Reference

3 so that only the major features are discussed here. Briefly, the enthalpy
of a specimen at a particular temperature was determined by dropping the
heated or cooled specimen into a cup which was maintained adiabatic. Enthalpy
was determined from the weight of the specimen and the temperature change
of the cup. The calorimeter cup was placed in an insulated container which
was immersed in a bath of ethylene glycol. Adiabatic conditions were main-
tained by heating or cooling the bath. The specific heat was calculated from
the slope of the enthalpy versus temperature curve. This slope was deter-
mined by averaging both a graphical solution and an analytical solution in
which the enthalpy curve was fitted by a least squares approach, and the
resulting equation differentiated to obtain the specific heat.
The temperature range of the adiabatic calorimeter equipment was

extended from -50°F to -250°F. This was accomplished by cooling the
specimen in a cooling chamber specially designed for inserting within the
standard cold box. The cooling chamber is constructed of two concentric
cylinders in which the specimen was inserted within the central cylinder,
and liquid nitrogen was placed in the annulus between the cylinders. With
this system, temperatures of -250°F were readily obtained. A continuous
dry helium purge was maintained eliminating any "frosting" on the specimen.
Ice calorimeter. - The drop type ice calorimeter employed to deter-

mine the enthalpy of the degraded material is fully described in Reference 4.
This calorimeter employed a cup surrounded by an ice mantle. The

enthalpy determinations were made by dropping the heated specimen into
the apparatus and measuring the volume of ice melted as the specimen
cooled to 32°F. Specific heat was calculated from the slope of the enthalpy
versus temperature curve.
Data and Results
Virgin material. - The enthalpy and heat capacity data of the virgin
material are included in Figure 9 and Table 4. The heat capacity values
increased from 0. 20 Btu/lb/°F (837 J/kg/°K) at -200°F to 0. 58 Btu'Ab/°F
(2427 J/kg/°K) at 600°F, with the values above 600°F becoming erratic
due to the excessive degradation of the material. The data up to 600°F
agreed well with the previous values obtained on the low-density phenolic-
nylon evaluated under Task Order 1. In comparison with the heat capacity
of phenolic-carbons, graphites, and silicas evaluated here previously, the
phenolic-nylon exhibited higher values. This was expected since the heat
capacity of nylon is significantly higher than that of carbon, graphite, or
silica.
Charred material. - The enthalpy and heat capacity data for the
charred phenolic-nylon are included in Figure 10 and Table 5. As shown
in the figure, the heat capacity increased from 0. 39 Btu/lb/°F (1632 J/kg/
°K) at 1000°F to 0. 57 Btu/lb/°F (2385 J/kg/°K) at 5000°F. This compares
favorably with the heat capacity obtained on the degraded phenolic-nylon
evaluated under Task Order 3, which remained a constant 0. 52 Btu/lb/°F
(2175 J/kg/°K) from 1200°F to 5000°F. As was expected, due to the
carbonaceous character of this material, the values obtained also com-
pared well with those of graphite (0. 4 Btu/lb/°F at 2000°F to 0. 55 Btu/
lb/°F at 5000°F for CFZ).
The scatter of the enthalpy data was relatively high due to the small
mass of the specimens; therefore, four specimens were evaluated in order
to reduce the uncertainty.
10
THERMAL EXPANSION
The thermal expansion of only the virgin material was determined

from -200°F to 750°F employing the precision quartz tube dilatometer.
A complete description of the quartz tube dilatometers is included in

Reference 3. Briefly, the specimen was placed in the bottom of a quartz
cylinder and a quartz rod placed on the specimen extended to the open end
of the cylinder. The thermal expansion was indicated by a precision dial
gage mounted to the cylinder with its stylus bearing on the rod. The speci-
men, which was heated in a tube type furnace, was instrumented with
thermocouples at three locations along its length to minitor temperatures
and temperature gradients. From calibration with standards such as "A"
nickel, the precision of the measurements has been confirmed within
0. 0001 inch scatter at any level and the total uncertainty within + 5%.
The cryogenic temperatures were obtained by two methods for

Specimens 1 and 2. The first was performed by immersing the quartz
dilatometer in a dewar filled with liquid nitrogen. The second utilized a
coil with several orifices drilled on the inside diameter which provided a
surrounding spray of the liquid and gaseous nitrogen on the outside of the
quartz tube. The second method provided better control of the tempera-
tures desired.
Data and Results
The thermal expansion data are shown in Figure 11 and Tables 6 and
7. Duplicate data were obtained in the direction perpendicular to the 4 inch
thickness defined as "ab" direction, and singular data from room temperature
to 750°F were obtained in the thickness direction defined as the "c" direction.
The determination in the thickness direction was not required under the
contract but was performed in order to determine if any anisotropy of
expansion existed in this material.
As can be seen from the figure, in the "ab" direction the material
expanded steadily from -200°F to 230°F at which point contraction occurred
and continued until 750°F. The coefficient of expansion in the "ab" direction
at room temperature was 23. 5 x 10"6 in./in./°F (42. 3 x 10-6 m/m/°K).
11
The expansion in the "c" direction, also shown in Figure 11, differed
from that in the "ab" direction above 150°F, being about 20% greater at
230°F. Above 230°F, contraction in the "c" direction occurred in a manner
similar to the behavior in the "ab" direction; however, above the cure
temperature (340°F) of the material, erratic data were obtained.
The difference in the observed expansions in the "ab" and "c" directions
may have been due to some anisotropy in the material, but more likely these
differences, particularly above the cure temperature of 340°F, were the
result of degradation of the material. We have noted with previous expansion
evaluations on reinforced plastics that erratic and unrepeatable data are
usually obtained above the material's cure temperature due to the spurious
thermal motions associated with degradation. More evaluations, which
were beyond the scope of this contract, would be required to fully define
the anisotropy that doäs exist.
In comparing the above values with those obtained on the phenolic-nylon

evaluated under Task Order 1, the prior phenolic-nylon exhibited expansions
about 10% higher over the range from -300°F to room temperature. From
room temperature to about 150°F the curves for the two materials were
almost identical. Above 150°F the prior phenolic-nylon also behaved
erratically but did not begin to contract until about 400°F.
PERMEABILITY
The permeability on both the virgin and charred materials was

determined at room temperature.
The apparatus employed for both virgin and charred material is

completely described in Appendix B. The procedure simply provides a
pressure drop across the specimen by mounting and sealing the specimen
between two chambers at different pressures. The flow of the permeating
gas through the specimen is monitored downstream from the specimen.
The measurement of the flow, specimen mean pressure, and pressure
drop across the specimen provided the data required to investigate the
permeability of the material. These data can be utilized in various
equations to provide permeability coefficients which are applicable for
various flow conditions. We chose to determine the admittance (Kmv)
defined in the equation
12
P
K -- mQm L
mv
AP A
where
2
Kmv = admittance, cm /sec
P = mean pressure in specimen
Q = flow rate through specimen, defined at mean pressure

cm3/sec
L s thickness of specimen, cm
2
A = cross sectional area of specimen exposed to flow, cm
AP = pressure drop through specimen
This admittance value is applicable to the combined Poiseuille (viscous)

and Knudsen (molecular) flows.
Permeating gases of helium and nitrogen were used in this investiga-

tion. Gas flow rates through the virgin material were measured with a
bubble flowmeter; the higher flow rates through the more porous char
material were monitored with a precision Rotameter made by Fischer
and Porter Company. Pressure differentials across the specimen ranged
from 1. 5 to 9. 8 inches of water. Two thicknesses (approximately 0. 25
and 0. 43 inches) of the virgin phenolic-nylon and only one thickness
(0. 25 inch) of the char were evaluated.
Data and Results
The pressure drop across, flow through, and mean pressure of both
the virgin and charred specimens are shown in Tables 8 and 9. The
calculated admittance is also included in the table to facilitate a comparison
of the data obtained under the various conditions foi the two materials.
13
Virgin material. - It was observed that for the virgin material the
admittance did not change (within the limits of uncertainty of the equip-
ment) with the two purge gases or with the variation in pressure differen-
tials across the specimen. However, some increase in values was noted
for the thicker specimens. The average values of the thinner Specimens
1, 4, and 5 were 4.15 x 10"4, 3.88xl0"4, and 4.10 x 10"4 m2/sec,
respectively; whereas, the average values of the two thicker specimens
were 4. 29 x 10"4 and 5. 07 x 10"4 m /sec, respectively.
Charred material. - For the degraded material, the admittance was

higher due to the cracked and porous structure and varied depending on the
permeating gas used and pressure gradient across the specimen. Nitrogen
provided lower values (approximately 0. 8 to 1. 0 m2/sec) than those exhibited
with helium (approximately 1. 4 to 1. 9 m2/sec),and there also was a drop of
20% in the admittance as the pressure drop across the specimen was increased
from 1. 5 to 3. 0 inch of water.
It is important to know the type of flow that occurs within the char in
studying the effectiveness of transpirational cooling during ablation. Due
to the size variations of the pores and channels within the material, the
type of flow will naturally vary between turbulent, transitional, and laminar
within the different passages. The data obtained on this char do indicate
that most of the flow was either transitional or turbulent. This was demon-
strated by the fact that the helium provided higher flow rates through the
char when compared with nitrogen. In a flow regime of mostly turbulent
flow, the volume flow rate is inversely proportional to the square root of
the gas density, and for laminar flow the flow rate is inversely propor-
tional to the viscosity. This can be seen from Darcy's equation (valid here
due to the low pressure drop) and was also illustrated by Creutz. Since
there is a wide variation in density (nitrogen 0. 072 lb/ft3; helium 0. 010
lb/ft3) and only a slight difference in viscosity (nitrogen 1770 x 107 poise;
helium 1960 x 107 poise) of the two gases, the higher flow of the helium
indicated that very little laminar flow occurred.
The same conclusion can also be drawn by applying the data to the
following relation offered by Creutz:
6
Qa(PAP)
where
Q z flow of gas through the sample (corrected for Knudsen and

slip flow rates)
14
P = mean pressure of the specimen
AP = pressure drop across the specimen
6 = exponent which is 0. 5 for turbulent and 1.0 for laminar flow
Using the data shown in Table 9, an approximate value of 6 can be

obtained by plotting Q vs (PAP) on logarithmic coordinates and determining
the slope, which is the exponent 6 . This was done, without correcting
for Knudsen or slip flow (which would be relatively small at these large
flows), and the slopes were about 0.9 for helium and 0.7 for nitrogen. This
value indicates the flow to be transitional. Therefore, for the pressure
drops between 1. 5 to 3.0 inches of water, the flow should be considered
transitional or turbulent for this char.
TOTAL NORMAL EMITTANCE
The total normal emittance of the degraded material from 1500°F

to 4000°F was determined. This was performed by comparing the irradiance
from the specimen to that from a cavity-type blackbody maintained at the
same temperature.
A complete description of the apparatus and procedure employed for

the emittance determinations is included in Reference 4. Briefly, the
specimen was heated in an induction furnace and its irradiance was moni-
tored by a 160^junction thermopile calibrated against a cavity type black-
body to about 5200°F. An optical pyrometer was employed to monitor
temperature of the specimen. The assumption of graybody emittance
and the use of the Wein and Stefan-Boltzmann equations permitted an
iterative calculation of true temperature and emittance.
Temperatures below 1500°F were not obtained since the irregular

surface of the char and its weak structure inhibited the proper contact
required for a surface thermocouple. Temperatures above 4000°F were
not obtained due to the destruction of the tungsten heating discs under the
specimen. The high heat flux and low conductivity of the char created a
very high temperature gradient across the specimen which accounted for
the melting of the tungsten disc while the specimen surface temperature
was about 4000°F.
15
The specimens were prepared by carefully cutting the discs (-^ inch
diameter by ^- inch to j inch thick) from the charred material. The top
surface of the char was unaltered from the as received condition and no
resin impregnant was used.
Data and Results
The total normal emittance data are shown in Figure 12 and Table 10.
The emittance increased slightly from 0. 79 at 1550°F to 0. 87 at 3300°F and
then decreased to 0. 79 at 4000°F. These values were, over most of the
temperature range, slightly lower than those obtained on the low-density,
phenolic-nylon char evaluated under Task Order 3. The significant
difference between the emittances of the two materials occurred between
the temperatures of 3000°F and 3500°F, where the emittance of the char
under Task Order 3 decreased due to the formation of a white residue.
The same residue was noted on Specimen 1 (see remarks in Table 10);
however, its effect on emittance was negligible for this char since the
amount of residue formed on the present specimens was probably less.
It was noted during the runs that the "speckled" appearance of the specimen
viewed through the optical pyrometer was not as noticeable for these runs
when compared with the runs performed under Task Order 3 indicating
less residue formation. Apparently the residue was formed by impurities
within the char as discussed in Reference 6.
Extra specimens were evaluated for emittance to obtain a represen-

tative mean due to the higher than normal data scatter which resulted
from the varying surface structure and the gray to black color variation.
The variation in the porous surface structure apparently caused different
degrees of subsurface radiation.
MECHANICAL PROPERTIES
On the nondegraded material, the tensile and compressive strength

properties in one direction were obtained from -200°F to 750°F. The
specific properties determined were ultimate strength, yield strength
at 0.2% offset, Poisson's ratio, Young's modulus, total elongation or
compression, and stress-strain curves.
16
The apparatus and procedures employed for the mechanical property

determinations are completely described in Reference 3. The specimens
were loaded in a Tinius-Olsen universal testing machine. Curves of stress
versus strain and lateral versus axial strain were continuously plotted to
failure on X-Y recorders. Strains were measured axially and laterally
in one direction. Triaxial strains were recorded during the initial tests
until it was confirmed that the material was essentially isotropic for this
property. Temperatures were obtained by programmed heating above 70°F
using tungsten filament radiation lamps controlled by a Powerstat. For
cooling, the specimen was surrounded by cotton sprayed with liquid or
gaseous nitrogen at a rate sufficient to provide the desired temperature.
The load was programmed to provide a given stress rate for failure at
approximately 5 minutes, thus the stress rates differed at different
temperatures. The strain in the direction of loading was measured by
dual "strain gage" clip-on extensometers mounted on lugs clamped to the
specimen. The strain in the lateral direction (perpendicular to the loading
direction) was measured by mechanical extensometers in contact with the
specimen which transmitted the lateral motion to a differential voltage
transformer.
This type of instrumentation provided precision recordings of the

load and the biaxial strains, continuously, to failure of the specimen. The
Young's modulus, ultimate strength, yield strength, Poisson's ratio, and
total elongation or compression were obtained from the curves.
The tensile specimens employed were 8-j inches long containing

a gage section l\ inches long by j inch wide by \ inch thick. The
compressive specimens were \ inch by TT inch in cross section by 1
inch in the loading direction.
Data and Results
Tensile properties. - All the tensile property values are shown in

Figures 13 and 14 and Table 11. Data were obtained to only 600°F since
burning of the specimens at higher temperatures caused premature
breaking. The tensile stress-strain curves, which are direct tracings
from the X-Y recordings, are included in Figures Cl through C22 of
Appendix C. Yield strength was not obtained on all runs in tension since
fracture occurred in most cases before the 0. 2% offset.
17
As can be seen from Figures 13 and 14, the tensile strength and
elastic modulus decreased with an increase in temperature, with a sharp
drop occurring between 200°F and 300°F. The ultimate strength decreased
from 570 psi (3. 93 x 106 N/m2) at -200°F to below 100 psi (0. 69 x 106 N/m2)
at 500°F. These values were about 50% lower than values obtained on the
low-density phenolic-nylon evaluated under Task Order 1. The lower
elastic modulus, yield strength and total elongation indicate the significantly
weaker structure of this material when compared with the previous low-
density phenolic-nylon. The weaker structure obviously resulted from the
formulation and processing being less than optimum for this material.
Considerable scatter was observed in the ultimate strength values

between -200°F and 200°F, and in elastic modulus and Poisson's ratio at
-200°F. This scatter may have resulted from several factors, such as
variations in stress rates (recall that these were varied to maintain the
loading period constant at about five minutes) or in the geometry of the
specimens which may have resulted in nonuniformities in stress and strain.
Unfortunately, time and funds did not permit an evaluation of these param-
eters; however, such a study will be performed on a low-density phenolic-
nylon of similar composition under a follow up task order (Task Order 4
under Contract No. NAS 1-5448).
The sharp drop in the strength and modulus above 200°F correlates
with the contraction at 230°F observed in the thermal expansion measure-
ments. Apparently the material undergoes a transformation above 200°F,
even though this temperature is below the cure temperature. Above the
cure temperature deterioration of the material contributed to the decrease
in strength. Typical photographs of the specimens after the run illustrating
the deterioration are shown in Figure 15. Also illustrated are the types of
fracture that occurred. The relatively flat breaks obtained did indicate
good tensile failure for most of the specimens.
Compressive properties. - All compressive property values are

shown in Figures 16 and 17 and Table 12. The compressive stress-strain
curves are included in Figures C23 through C48 of Appendix C. Some of
these curves are direct tracings of the X-Y recorder; however, the others
were plotted since the lateral strains were obtained on a recording oscillo-
graph.
As shown in Figures 16 and 17, the strengths and moduli decreased

steadily with an increase in temperature. The ultimate strength decreased
from 2600 psi (17. 93 x 106 N/m2) at -200°F to approximately 200 psi (1. 38 x
106 N/m2) at 750°F. As was the case with the tensile properties, these
values were considerably lower (again by approximately one-half) than
18
those exhibited for the previous phenolic-nylon evaluated under Task Order 1.
As did the tensile strengths, the compressive strength values exhibited
considerable scatter below 200°F. The elastic modulus and Poisson's ratio
values were also scattered, though not as much as the values measured in
tension. Further studies are needed to isolate variations in the test methods
from those inherent in the material.
DISCUSSION OF RESULTS AND A COMPARISON

WITH PROPERTIES OF PRIOR PHENOLIC - NYLON
Some correlation of the properties can be made from a review of

the data. For purposes of comparison, comprehensive plots of the proper-
ties of the virgin low-density phenolic-nylon are presented in Figures 18
and 19. Properties of the prior low-density phenolic-nylon^ evaluated under
Task Order 1 of Contract No. NAS 1-2978, are also shown.'
Reference to Figure 18 shows that the thermal conductivity of the

phenolic-nylon evaluated in this task order ranged from 7 to 23 percent
lower than that of the phenolic-nylon evaluated under the prior Task Order
1. As discussed earlier, the lower conductivity may have resulted from
the high percentages of filler and poorer bonding between resin and filler
in this material. The characters of both curves were similar, both exhibiting
a sharp peak in the vicinity of -100°F. The reason for this peak, which is
about 30 percent higher than the values on either extremity, is not known.
The enthalpies of the current and prior materials were essentially *

the same.
The thermal expansion of the current phenolic-nylon was lower than

that of the prior material over the temperature range from -300°F to 150°F.
Both materials exhibited erratic behavior above 150°F.
Figure 19 shows composite plots of the mechanical properties of the

current and prior (Task Order 1) phenolic-nylons. The ultimate tensile
and compressive strengths of the current material were about 50 percent
lower at -200°F than those of the prior material but decreased less with
temperature, so that at 600°F the two materials exhibited about the same
strengths. The tensile modulus exhibited a rather sharp decrease at
200°F (recall that thermal expansion exhibited a reversal near 200°F).
The moduli were lower than those of the prior material from -200°F to 200°F
and about the same at higher temperatures.
19
Figure 20 shows a composite plot of the thermal properties of the
low-density phenolic-nylon char. For comparison, data are presented
for a high-density and a low-density phenolic-nylon char evaluated under
prior Task Orders 2 and 3, respectively, of Contract No. NAS 1-2978.
Observe that the emittance of this char remained more nearly

constant with temperature than that of the prior low-density char, but was
slightly lower over most of the temperature range.
The thermal conductivity of this char was lower than that of either of
the prior chars. As expected, the characters of the three curves were
similar with the values increasing rapidly with temperature due to radiation.
The differences in the conductivities of this and the prior low-density char
can probably be attributed to differences in microstructures, even though
the densities and porosities of the two materials were about the same. The
current material was more heterogeneous, containing areas of relatively
dense char separated by large voids (see the prior Figure 3). The median
pore size, which is probably more representative of the relatively dense
areas than the mean pore size, was 18. 2 microns. Reference to Figure 4
shows that the majority of the pores are clustered around this size. On
the other hand, the prior low-density char was more uniform in appearance,
exhibiting few large voids. The average pore size of the prior material
was also larger at 24. 2 microns. At higher temperatures, radiant heat
transfer would be larger through the char having the larger pore size,
other factors being equal. At lower temperatures differences in conductivities
could result from such factors as degree of graphitization of the matrix.
X-ray diffraction patterns, not obtained in these programs, might detect
such differences.
The current low-density char also exhibited the lowest enthalpy of

the three chars, although the heat capacities of the two low-density chars
were about the same. The heat capacity of the high-density char increased
more with temperature, being about 20 percent greater at 4000°F than that
of the low-density chars.
Southern Research Institute

Birmingham, Alabama
February 24, 1967
20
REFERENCES
1. Wilson, R.Gale: Thermophysical Properties of Six Charring Ablators

from 140° to 700°K and Two Chars from 800° to 3000°K. NASA
TN D-2991, October 1965.
2. Keller, L. B. : Development of Characterized and Reproducible

Syntactic Foam of Phenolic-Nylon for Heat Shields. NASA CR-
73041, 1966.
3. Pears, C. D.; W. T. Engelke; J. D. Thornburgh: The Thermal and

Mechanical Properties of Five Ablative Reinforced Plastics from
Room Temperature to 750°F. AFML TR 65-133, April 1965.
4. Pears, C. D. and J. G. Allen: The Thermal Properties of Twenty-

Six Solid Materials to 5000°F or Their Destruction Temperatures.
ASD TDR 62-765, August 1962.
5. Creutz, E. : Laminar, Turbulent, and Transition Gas Flow in Porous

Media. Nuclear Science and Engineering, vol. 20, 1964, pp. 28-
44.
6. Pyron, CM., Jr.; and C. D- Pears: Some Thermophysical Properties

of a Low-Density, Phenolic-Nylon Char. Final report under NASA
Contract NAS 1-2978, Task Order 3, January 1965.
21
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29
Temperature - °K
33 144 255 366 477 589 700
."'.'. - t. x......jr..-- -j^-.-t T ~f - -- i-j_- - -x ■■ ■ ■ 2511

0.60
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(4 .i.X ..Ü)Xi"...- ....._. -f Mathematical curve fit u
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evaluated under contract ~-
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a NAS 1-2978, Task Order 1 , '1114T , 7XXX '
! U|.|i 14! | | J | !.| j-141-1 j |4 i-4 (T in degrees R) J.
0.00
-400 -200 200 400 600 800
Temperature
Temperature - °K
33 144 255 366 477 589 700
Enthalpy 4V ..| p ... f..".. ::.r;::./4
O Specimen 1 - 4j_ i ^ f V.:4."/. <
300 - D Specimen 2 —Excessive charring- *«j^ ~fK... Z1 698
A Specimen 3 -T - 4 — 3f"T5
Q Specimen 4 -- -f-t— - ,P -
_— -, e 7
<u
u [7 Specimen 6 —44 Xp
c 465
<P
200
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HI
to
o
in -+- Least squares curve fit h/ "3o
00
(from -50 F to bOO v) 9 ~ t' 233
100 hg5 = 0.15T + 2.1 x 10 1 - /
1-3
3 + oöyTT + 14o .)(*- r

ffl
m
-- — — - jt a
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-100 ■ ■Tl 1 MQ JJ---XL----J-----^7/TYrTftTTI 1 TIT IT t 111111 mi 111 -233
-400 -200 200 400 600 800
Temperature - °F
Figure 9. Enthalpy and heat capacity of the virgin low-density phenolic-nylon
30
Temperature - °K
2477 3033
0 «
&
1.0 4184 M
J«
~3
4-»
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o
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ri 2092
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Temperature
2500
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a N^ - 'v -■- - A Specimen 3 a
rt
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"4- T.paRt RmiprpR solution
I
W
C w
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X X r n32 s U. 4oT + 1.8x10 »T +_
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.■ds::.^.!!!..., L 1 II 1 M ! M ! M 1 1 II 1 1 1 I! 1 1 1 1 1 1
1000 2000 3000 4000 5000 6000
Temperature
Figure 10. Enthalpy and heat capacity of the low-density phenolic-nylon char
31
Temperature °K
144 255 366 477 589 700
s
a
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o
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ro
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200 400 600 800

Temperature - °F
Figure 11. Thermal expansion of the virgin low-density phenolic-nylon
32
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Temperature - °K
33 144 255 366 477 589 700
l i: ■ ii'f: :jF 7lt ffft v ::itl"lTtf" ::i f f|--)f{-:-"4-'-"-::'

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Temperature - "F
Figure 13. Ultimate tensile strength versus temperature for

the virgin low-density phenolic nylon
34
Temperature - °K
144 255 366 477 589 700
g 0.40
o
0.20
-400 -200 200 400 600 800

Temperature - "F
Temperature
366 700
250 11724. 7
200
o 150
.5
01
■—i
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3
■O
1 100
-400 -200 200 400 600 800

Temperature - °F
Figure 14. Initial elastic modulus and initial Poisson's ratio loaded in
tension versus temperature for the virgin low-density phenolic-
nylon
35
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144 255 366 477 589 700
~. 2500 17.24
00
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2000 13.78
10.34
S 1500
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1000
1
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500
-400 -200 0 200 400 600 800

Temperature - °F
Figure 16. Yield and ultimate compressive strength versus temperature

for the virgin low-density phenolic-nylon
37
Temperature - °K
33 144 255 366 477 589 700
o ^
... _ _ .
Initial Poisson's ratio
. ,J
7
ß 0.40 z
§m
e JL
0.20 ::::::::: jt::: JE::::-::S:::::nt---3f:::-«::::::::::::::::::

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-400 -200 200 400 600 800

Temperature - °F
Temperature °K
33 144 255 366 477 589 700
a :: ; i i1034.2
150
_-
_, Initial elastic modulus
a
1o 100 :: ::_jiL_Ü5sir
S
-_ 689.5
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oL J-
-400 -200 200 400 600 800
Temperature - "F
Figure 17. Initial elastic modulus and initial Poisson's ratio loaded in
compression versus temperature for the virgin low-density
phenolic-nylon
38
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39
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Temperature - *F
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1500 .'^. _ ^ Lk J,^. . Low-density phenol e-nylon
.. _: J^ 'jf '/[- / -jJP " = - evaluated under Task Order 1
... ----- y/': ?$L#¥:M.'±q- y;.\-- ■::::"$.-:...:.:::::;;::::::::

■ - -■ -- >{■ -- -V-? a-- 'ir ■ - ip---
j_- - - --y h V A . J...- ...-.£
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Ultimate tensile strength f/t- ; . t „._:;£ ?&££ l£*^ SS& >i -"*"■ ■-
-400 -200 0 200 400 600 600

Temperature - "F
ilffiffl
nitial elastic modulus
%
Yi Compressive modulus of low-density
phenolic-nylon evaluated under TaBk
Order 1, Contract NAS 1-2978
j Tensile modulus of low-density,
] phenolic-nylon evaluated under
j Task Order 1, Contract NAS 1-2978
Figure 19. Composite plot of mechanical properties of nondegraded low-density

phenolic-nylon
40
1.0
ll i
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1 lili liil ill Uli ilk &K? Wk ij/Uii , 111 I '
Low-density char evaluated under J\
prior Task Order 3 (Contract NAS 1-2978)1
... #1.11 l-Hl
'. Low-de isity char evalua led
It '1
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TC ^ T under c jrren Task Orde r 4
t
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Temperature - "F
80
If
e
8 T:-:-;:-^;-;r :r::r-::;::;::i:::;:r':::V^ -;l::;p^:^::|':::::'f'rti'.:^;|f .'
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1 evaluated under prior Task Order 3 - - -
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1 r :
Iv|l|i^- ::: ->|jEi|S"iäiSS „iW"^. - M - ^ Low-density char (p ■ 0. 24 g/cc)
E i t fr'■■■■ ' ijamS-tfrîtrf^tj lkUI$%.:f^.:i k-kik

-1- 1 . r T A- High-density char (p= 0.36 g/cc) .. -....... .
s 1 Tli If it 1 FT' ITT'
Thermal conductivity - | - | - \- ^ evaluated under p rior Task Order 2 -t 1. _ -| _ . .. -
-iTm-i ; i i i i i i i i i i i r „jl'l; , ; ' 1 i i i I I i i i i i i rrrr iriii;iiIIIIiI I I 1 1
Temperature -
;| - i: - . f. ; :. ' \:..
! }■1 ... ).:. J I" . -. 'A... . : |j ". -f |- [ HI. :.: : l

■[-■■- 4 ...... . . . ^ 1
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.."^^.'ft ■■■—-t - f -- ! !.t!!|!|.;:|;r|;j|:r-- .■-. J

i --.-■■-)- -.
0 1000 2000 3000 4000 5000 6000 7000
Temperature - *F
W 1000
1000 2000 4000 5000

Temperature - aF
Figure 20. Composite plots of the thermal properties of the low-density phenolic-nylon chars
showing comparison with prior chars
41
TABLE 1
DENSITY VARIATION WITH TEMPERATURE OF THE

VIRGIN LOW-DENSITY PHENOLIC-NYLON
Temperature Density
°K kg/m3 lb/ft
-200 144 596 37.2

■100 200 592 36.9
0 255 589 36.8
75 297 586 36.6
100 311 585 36.5
200 366 579 36.1
^Calculated from density values measured at room temperature and

measured coefficients of thermal expansion.
42
TABLE 2
THERMAL CONDUCTIVITY OF THE VIRGIN LOW-DENSITY PHENOLIC-NYLON
Average
specimen Total heat Average Specimen thermal Specimen thermal Time at
mean input specimen AT conductivity in 10~B conductivity temperature
watts op Btu/sec/ft/°F W/m/"K hour
temperature - *F
Specimen No. 1
Gum Rubber Filler
-241.6 4.82 43.6 1.25 0.078 5.0
-87.6 6.95 44.0 1.78 0.111 5.0
-13.5 9.21 93.1 1.12 0.069 5.0
118.3 5.20 45.9 1.28 0.080 5.0
Fiberfrax- Gum
Rubber Filler
182.3 9.08 87.2 1.17 0.073 4.0
359.4 27.80 230.6 1.36 0.085 4.5
398.8 16.25 136.7 1.34 0.084 5.5
547.0 25.17 195.2 1.45 0.091 4.8
606.0 30.45 223.0 1.54 0.096 14.0
821.8 44.78 293.5 1.53 0.095 6.5
Specimen No. 2
Gum Rubber Filler
-202. 2 4.70 39.9 1.35 0.084 6.0
-101.6 6.52 48.1 1.55 0.097 5.3
-20.1 5.86 80.7 1.35 0.084 4.5
117.0 5.42 46.2 1.34 0.084 18.0
Fiberfrax - Gum
Rubber Filler
168.5 9.07 76.2 1.36 0.085 6.0
324.8 26.23 201.8 1.43 0.089 18.5
362.7 16.73 129.3 1.42 0.088 6.5
490.7 24.48 170.0 1.49 0.093 16.0
592.4 30.63 209. 3 1.47 0.092 7.5
594.8 30.52 211.7 1.45 0.090 22.7
714.8 37.28 259.5 1.31 0.082 8.3
Central diameter = 4.0 inches

Specimen thickness
Specimen 1 s 0. 2493 inch prior to run 0. 2216 inch after run
Specimen 2=0. 2529 inch prior to run (no-change observed to 325°F)
= 0. 2439 inch at 324. 8°F + 3% )
a 0. 2421 inch at 362. 7°F + 3% [ Thickness estimated from monitoring thickness
= 0. 2289 inch at 490. 7°F + 7% V* change by measuring the gap spacing between
= 0. 2221 inch at 592. 4°F + 8% I the hot and cold face of the specimen.
= 0. 2217 inch at 594. 8°F + 8% J
z 0. 2015 inch at 714. 8°F - measured after run with micrometer.
43
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50
TABLE 5
ENTHALPY OF THE LOW-DENSITY

PHENOLIC-NYLON CHAR
Specimen
number Drop Initial Final Enthalpy from drop
and run temperature weight weight temperature to 32°F
number op grams grams Btu/lb
Specimen 1
Run 3 1025 1.165 1.095 101.5
6 2050 1.245 1.235 642.8
7 2550 1.290 1.275 784.5
8 3075 1.310 1.240 1305.9
9 3505 1.245 1.245 1415.5
10 4075 1.240 1.235 1645.4
11 4555 1.275 1.250 1549.5
Specimen 2
Run 5 1985 1.280 1.265 502.0
6 2540 1.205 1.195 916.7
8 3500 1.250 1.230 1316.5
11 4920 1.290 1.230 2452.4
12 5055 1.220 1.210 2296.1
Specimen 3
Run 2 2520 1.230 1.215 823.2
3 3055 1.255 1.230 1381.1
4 4520 1.265 1.230 1923.2
Specimen 4
Run 1 1497 1.235 1.255 227.7
4 3020 1.195 1.185 1018.2
5 4140 1.180 1.185 1473.7
6 5025 1.230 1.205 2358.3
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TABLE 8
PERMEABILITY OF VIRGIN LOW-DENSITY

PHENOLIC-NYLON AT ROOM TEMPERATURE
,
Admittance
Specimen Pressure Flow rate of gas Kmv ..
number drop across Mean pressure at bubble
and Purge specimen of specimen gage cm /sec or ft /sec
thickness gas in. of water in. of water cm.3/sec 10"^n2/sec
Specimen 1 nitrogen 2.50 408.05 .1100 4. 2078 .00453

0. 263 inch 5.50 409. 55 .2411 4.1922 .00451
5.60 409.60 .2450 4.1839 .00450
9.75 411.68 .4214 4.1333 .00445
9.75 411.68 .4184 4.1038 .00442
helium 2.50 408.05 .1062 4.0624 .00437
2.80 408. 20 .1210 4.1327 .00445
5.60 409.60 .2465 4. 2095 .00453
5.30 409.60 .2381 4. 2962 .00462
9.60 411.60 .4077 4.0614 .00437
9.60 411.60 .4120 4.1042 .00442
Specimen 2
0. 4218 inch helium 2.60 408.10 .0739 4.371 .00470
2.70 408.15 .0782 4.454 .00479
5.60 409.60 .1613 4.430 .00477
5.60 409.60 .1647 4.523 .00487
9.60 411.60 .2740 4.390 .00472
9.70 411.65 .2809 4.454 .00479
nitrogen 2.50 408.05 .0733 4.509 .00485
2.70 408.15 .0703 4.004 .00431
5.50 409.55 .1563 4.371 .00470
5.60 409.60 .1468 4.032 .00434
9.60 411.60 .2483 3.978 .00428
9.60 411.60 .2475 3.965 .00427
Specimen 3
0. 4334 inch nitrogen 2.65 408.13 .0812 4.905 .00528
2.70 408.15 .0851 5.045 .00543
5.65 409.63 .1798 5.094 .00548
5.75 409.68 .1808 5.033 .00542
9.60 411.60 .3003 5.007 .00539
9.70 411.65 . 3086 5.093 .00548
helium 2.50 408.05 .0805 5.154 .00555
2.50 408.05 .0793 5.077 .00546
5.75 409.68 .1852 5.166 .00555
5.75 409.68 .1855 5.164 .00556
9.40 411.50 .2907 4.950 .00533
9.55 411.58 .3067 5.141 .00553
54
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56
TABLE 10
TOTAL NORMAL EMITTANCE OF LOW-DENSITY PHENOLIC-NYLON CHAR
Observed Radiometer True

temperature output temperature
Time °F millivolts °F Emittance Remarks
Specime n 1
3:53 1468 0.198 1551 0.77 Attempted to run at
3:58 1463 0. 206 1540 0.81 higher temperature
4:05 1561 0.256 1649 0.82 (approx. 3200°F)
4:15 1865 0.482 1985 0.86 but radiometer sig-
4:24 2326 1.139 2485 0.95 nal became noisy.
4:38 2710 1.835 2940 0.85 White coating on
4:44 2720 1.818 2960 0.82 surface noted dur-
ing disassembly.
Specimen 2
9:21 1480 0.199 1566 0.75
9:29 1910 0.490 2047 0.79
9:35 2280 0.954 2460 0.82
9:45 2840 2.336 3059 0.94
9:53 3305 3.986 3591 0.90
10:03 3480 4.763 3796 0.88
Specime n 3
1:13 1526 0.235 1611 0.81

1:23 1875 0.461 2007 0.79
1:32 2333 1.030 2521 0.82
1:38 2720 1.810 2961 0.82
1:45 3199 3.605 3463 0.93
Specimen 4
9:38 1448 0.19£ 1524 0.81
9:44 2015 0.600 2164 0.80
9:50 2286 1.043 2447 0.92
10:00 2772 2.094 2991 0.91
10:05 3330 4.339 3585 0.99
Specime n 5
I
10:18 | 3480 4.721 3802 0.87
Specimen 6
1:16 I 3605 4.954 4008 0.76
i
1
Specimen 7
9:45 | 3005 2.622 3286 0.87
Specimen 8
2:43 2895 2.396 3139 0.88
2:48 3143 '3.057 3451 0.80
2:53 3262 3.441 3600 0.77
3:06 3535 4.681 3913 0.78
57
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59
APPENDIX A
DETAILED MATERIAL DESCRIPTION
The following detailed description of each constituent within the

low-density phenolic-nylon was supplied by the NASA Langley Research
Center.
Union Carbide BRP-5549

Phenolic Resin
The properties of the resin as published by the manufacturer are

shown in the table below
Property Property value
Density £3
16. 8 to 19. 4 lb/ft
(270 to 310 kg/m3)
Sieve Analysis
(U.S. Std. Mesh)
on 40 mesh 0. 0%
on 100 mesh 0. 6%
on 200 mesh 2. 0%
through 200
mesh 98.0%
Hexamethylene 8. 7 - 9. 5%
tetramine
content
Measurements with a Coulter Counter (Coulter Electronics

Industrial Division) at the Langley Research Center indicate that the
range of diameters of the phenolic resin powder particles is 0. 0001 to
0.0048 in. (2 to 120 /urn) with about 80% by volume of the powder having
diameters ranging from 0. 0003 to 0. 0023 in. (6 to 58 ßm).
60
Phenolic Microballoons
The properties of the Microballoons as published by the manufacturer

are given in the following table:

3
Density (liquid displacement 15. 6 lb/ft3 (250 kg/m )
Density (air displacement) 18. 7 lb/ft3 (300 kg/m3)
Flotation in toluene dupanol
solution Not less than 90% must float
Average particle size (dia) 0.0017 in. (43 /urn)
Size range (dia) 0. 002 to 0. 0005 in. (13 to 51 ßm)
Measurements with the Coulter Counter indicate that the range of

diameters of the phenolic Microballoons is 0.0004 to 0.0100 in. (10 to
250 /um), with approximately 85% by volume of the Microballoons having
diameters ranging from 0.0024 to 0.0080 in. (60 to 200 jum).
Nylon
Properties of the nylon powder as given by the manufacturer are

listed in the table below:
Specific Gravity 1.3 - 1.15

Melting Point 482 - 500°F (523 - 533°K)
Tensile Strength 11, 800 psi (81. 4 MN/m2)
Coefficient of Linear
Thermal Expansion 45. 0 x 10"6 in./in. - °F
(81.1 xlO-6 m/m- °K)
Thermal Conductivity 1. 31 x 10"*Btu-in. /ft2-sec-°F
0.068 W/m - °K
Specific Heat 0. 3 - 0. 5 Btu/lb - °F
1.25 to 2.09 kJ/kg - °K
Preliminary studies using a Coulter Counter indicate that about

85% by volume: of the nylon powder lies in the range from about 0. 0012
to 0. 0157 in. (30 to 400/j.m) in diameter, with about 5% below 30 jum and
10% above 400 ju.m.
61
APPENDIX B
APPARATUS FOR THE DETERMINATION OF PERMEABILITY
The flow of gas through a material can be of two different types,

Knudsen (molecular) flow which is governed by the relation
Km (AP) A-T/KT
q = —
PL (1)
l
and Poiseuille (viscous) flow, which is described by
q= K„ (AP) ifo + Pj A
PLn
where
q = volume flow rate measured at absolute pressure P

AP = pressure drop across the specimen
A = area of the specimen normal to the flow of gas
L = length of the specimen parallel to the flow of gas
R = gas constant of the gas
T = absolute temperature
rj = viscosity of the gas
§•2 (P2 + Px) = average absolute pressure on the specimen
K-y,
K = molecular permeability coefficient
K" = viscous permeability coefficient
For those cases where neither equation fully describes the gas flow, the
flow is both molecular and viscous and the expressions for both types of
flow are combined which yields:
AAP
q r (Ko ^HRT + K, _EL )
1 PL (3)
*Barrer, R. M. , Diffusion In and Through Solids, Cambridge University

Press, Cambridge, pp 60-61, 1951.
62
where K„ and Kx are permeability coefficients similar to Km and Kj,,
respectively, and P = j (P2 + Pj.
To evaluate the coefficients KQ and K:, let
n (4)
Equation (3) may then be written ■":
q = K m i> AAP
PL (5)
or
Kmv = PL3-
AAP (6)
Km[;, often called the admittance, can then be determined for the specimen
at any pressure by measurement of the flow rate q at that pressure. Values
of KmJ, for several different pressures can then be plotted versus Pm and,
as seen from equation (4), the resulting line will have a slope of I^/n
and a zero intercept of K^, l) RT. Thus, Kx and K„ can be determined
from the properties of the gas used.
If metric units are used throughout equation (3), K0 will be in cm and

2
Kx in cm .
These coefficients should be dependent only on the structure of the

material; that is, independent of specimen configuration, viscosity and
molecular weight of the gas, temperature, pressure gradient, and the
average pressure.
The data required to calculate the admittance (Km ) are pressure at

the flowmeter (P), indicated flow rate at the flowmeter (q)> thickness of
specimen (L), area (A), and pressure drop across the specimen (AP).
For cases where the temperature of the specimen is at room temperature
or the same temperature as the flowmeter, the product of Pq measured
at the meter is equal to the product Pq at the specimen, since from
continuity
63
W r p AV = p q = constant (7)
For a perfect gas,
p =
RT~ (8)
Therefore, from (7), equating conditions at the specimen and the

flowmeter
Ps%=Pmqm (9)
where the subscripts s and m refer to the specimen and meter, respectively.
Substituting from (8)
<10)
—
RTS
«. = ^r-
RT„,
i«
Therefore, for isothermal flow
p
s qs = Pm qm <n>
If the temperatures at the specimen and meter are different, then the
term Pm qm (Pq in equation 6) must be multiplied by the ratio Ts .
T
A schematic of the apparatus being used for the determinations of the

permeability coefficients is shown in Figure 1. The primary side of the
specimen is exposed to desired gage pressures which can be measured by
a laboratory gage or a U tube manometer. Since the secondary side of
the specimen is exposed to atmospheric pressure or a known pressure, the
pressure drop across the specimen is readily obtained. The flow of gas is
measured at the exit side of the specimen with either a bubble flowmeter,
for which a stopwatch is employed to measure the displacement time of a
soap bubble, or a wet test flowmeter. The bubble flowmeter operates at
atmospheric pressure, and the wet test meter operates at a slightly higher
pressure which is monitored.
64
For specimen materials that can be machined with good tolerance,
the brass assembly containing the specimen is shown in Figure 2. The
1 inch diameter x j inch thick specimen is placed on the •gj inch shoulders
and sealed by filling the annulus around the specimen with the sealer material.
For porous and weaker structured materials, the specimens are mounted and
sealed in the brass assembly shown in Figure 3. For this assembly, the
specimens can be roughly machined in the form of a disc of approximately
1 inch diameter.
Several types of sealants were investigated for room temperature use

with Dow Corning Silastic RTV 731 giving the best results. This material is
viscous and can be applied easily. It wets the specimen well and provides an
excellent seal after curing to a solid rubbery form. The system is thoroughly
purged before securing the specimen assembly.
65
in
3
u
m
a.
a
<
■3
D
e
<u
a,
ID
XI
J3
O
a)
3
OB
fa
66
Primary Chamber
Specimen
RTV 731 Sealant
O-ring
Secondary Chamber
ton
Figure B2. permeability Specimen Assembly
67
Primary Chamber
(Brass)
Specimen
Retainer Ring \
RTV 731 Sealer

Specimen Holder
(Brass)
O-Ring
Secondary Chamber
(Brass)
Figure B3. Permeability Specimen Assembly
68
APPENDIX C
STRESS-STRAIN CURVES IN TENSION AND COMPRESSION
69
400 17.25
320 13.80
in
a
a 5
si
& 10.35
c n
I

6.90 U
a
u
■*->
a
3.45
8.12
Axial strain in 10 in. / in.
Figure Cl. Axial tensile stress-strain and bi-directional

strains at 70°F for a virgin low-density phenolic-
nylon
70
Temperature - 70°F
610 - " _
" ■ ------ Crosshead rate - 0. 02 in. /min _ 20.55
Ultimate strength - 538 psi
/
z 1
^Cf--Stress v.3 axial strain
400 _ _. '-j • 16.44
01 ,f
a j
.'
.5 7
■
/
-j
1
' o
ff j
u *>DU / 12.33 .3
r
7
.
~i
t I
.'
/
\ «j
OAA -J u
8.22
" j -
/r
j ■
r
^
/
122 * 4.11
\
/ 7 'E = 7«n 0 x 1U psi
/ y* II II
t\ ,/ 1
^P» *J^y 1 1
/ — M ^"" ê 1 T i. 1
vs axiaj strain • 1 L
j
#
0 """ ^-—-—Initial Poisson's rati 0 =,0.14 : ±
3.95 7.90 W.M 15.80 19.75 23.70
Axial strain in 10" in./in.

Figure C2. Axial tensile stress-strain and bi-directional strains at 70*F
for a virgin low-density phenolic-nylon
71
1 1 1 1 1 1 1 1 1 1 1 I I ( I I I I ; j | | | j | j_
■ _ . . — ~~ 1 — ■
-
Specimen run T-o
Temperature - <u x1
Time
. ,
to rupture
,
- *|i min
TV\{M
_
Ultimate strength - 571.6psi-- 20.55

610 .
j i
L
J
/
"j
16.44
488
0)
/
J
j _L
_1_
_ . . - 4
a _E_^__ _
_. . . .3
.3 ...... J n
12.33 S
Ji —
-4-*
60
a 366 j
u I
. , „ jr
CO
J
0) " J _
.......J
to f"
2 ■ 8.22
2<u 244 f u
J
(U ...... r
nJ
S /
A 3
1
T _ . .
- - §
/ _ 1 ■ 4.11
122
- J--*--E= 83.4x10 psi
:-£-. - :::~:::::p: TT
_y h=-= Lateral vs axial strain
^ffla^fflTOttmtmtmtttttlfflffiT^S^
3.95 7.90 11.85 15.80 19.75 23.70
Axial strain in 10"3 in./in.
Figure C3. Axial tensile stress-strain and bi-directional strains at 70°F for a
virgin low-density phenolic-nylon
72
■
Specimen run T-6

Temperature - 200°F 20.55
610 " ~ " *" ~ ~ — A r\
Time to rupture - 4.9 min
_ , , . f\ AP . /
Crossnead rate - u. Uo in. /mm
j^ i j
f
t*
4ÖÖ * 16.44
j ti ]
>tress vs axial strain
. , . .5
,r i
J(J
;*
j *
* | ■
©
« .» J^
n
366 ~ "+" y 12.33
n J
?
■ r'
.f
r .
f\ |~
j
/ l (
244 " _._.r

jf
jrl ... _. T" . ." 8.22 t
ID
/
r
* 3
. //
J 3 . . _ . .. _ .
4.11
J ^ —1 J 1
y ^ -I i- ^îr . _
-■ /U^j h JX.--^jT_.*v
■ 1 j i j i 1 1 j i
yJ i i t ^^^«■ *" "^ i1 1 | [ | j |
r ]_.x.-■* j'Lr* T ... i -n * i ■
LLJ- 11 1 i -LJ 1 1 1 1 1 1 i 1 1 1 1 1 1 I.11J |>| i __U L-j-
3.95 7.90 11.85 15.80 19.75 23.70 27.65
Figure C4. Axial tensile stress-strain and bi-directional strains at 200°F for a virgin
low-density phenolic-nylon
73
~-
—
"
Specimen run T-7

Temperature - 200°F -=-
l
Time to rupture - 3 min —
20.55
610 Crosshead rate - 0.05 in.^nin—
-\--- - Ultimate strength - 553 psi
, .I -J
Ä-
_.. X- - - -
16.44
488 ., u
ft
.3
-/- —■
—r,
si o
" " "" f
ß /
i
12.33 .3
366 r
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122 —4—
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r j* Lateral vs axiai strain

1 <m —
.___ J-J n1
N
±n±t±Ji±L-
■
.... . _. ....
Initial Poisson's ratio z 0.14 -- \-
3.95 7.90 11.85 15.80 19.75 23.70 27.65
low-density phenolic nylon
74
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Figure Cl4. Axial tensile stress-strain and bi-directional strains at 300°F for a virgin
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Axial strain in 10~3 in./in.
Figure Cl7. Axial tensile stress-strain and bi-directional strains at 0°F
86
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Figure Cl9. Axial tensile stress-strain and bi-directional strains at -200°F for a
virgin low-density phenolic-nylon
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Figure C20. Axial tensile stress-strain and bi-directional strains

at -200°F for a virgin low-density phenolic-nylon
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Figure C22. Axial tensile stress-strain and bi-directional strains at -200°F
91
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NASA CONTRACTOR NASA CR-809

NATIONAL AERONAUTICS AND SPACE ADMINISTRATION WASHINGTON, D. C. JULY 196

THERMOPHYSICAL PROPERTIES OF A LOW-DENSITY

PHENOLIC-NYLON ABLATION MATERIAL

By W. T. Engelke, C. M. Pyron, Jr.,

Distribution of this report is provided in the interest of

Prepared under Contract No. NAS 1-2978 by

for Langley Research Center

NATIONAL AERONAUTICS AND SPACE ADMINISTRATION

^i-'-'ii-t'.i'X'i''" IM. ~^":~'ri:p~Tr

LOW-DENSITY PHENOLIC-NYLON ABLATION MATERIAL

Some physical properties were determined on a low-density phenolic-

The low-density phenolic-nylon was a molded composite consisting

The thermal conductivity of the virgin material from -200°F to 750°F

The thermal conductivity from 1000°F to 5000°F of the charred material

The heat capacity of the virgin material increased from 0. 20 Btu/lb/°F

The mechanical properties of the virgin material from -200°F to 750°F

This is the final report on the thermophysical property evaluation of

Specifically, the thermal conductivity, heat capacity, thermal expansion,

The low-density phenolic-nylon material was supplied by the NASA

This low-density phenolic-nylon composite was molded and consisted

A more thorough description of the individual constituents is included

To further define the as received material, the densities of both the

A micrographic evaluation was also performed on the char to deter-

The thermal conductivity was determined in one direction (thickness

Apparatus and Procedure

Basically this apparatus consisted of a central heater plate surrounded

During the run on Specimen 2, the change in thickness at the higher

Radial inflow apparatus. - To determine the thermal conductivity of

Briefly, the test section was heated radiantly in a high temperature

To measure the thermal conductivity of the char specimens, the

The machining of the conductivity specimens was performed after

Virgin material. - The thermal conductivity data for the virgin

Charred material. - The thermal conductivity values of the charred

k = 11.57 x 10_5 +5.3 x 10"15T3 (2)

k z thermal conductivity, Btu/sec/ft/°F

T = mean temperature of specimen, °F

Two apparatuses were used in the determinations. For the evalua-

Apparatus and Procedure

Adiabatic calorimeter. - This apparatus is fully described in Reference

The temperature range of the adiabatic calorimeter equipment was

Ice calorimeter. - The drop type ice calorimeter employed to deter-

This calorimeter employed a cup surrounded by an ice mantle. The

Data and Results

The thermal expansion of only the virgin material was determined

Apparatus and Procedure

A complete description of the quartz tube dilatometers is included in

The cryogenic temperatures were obtained by two methods for

Data and Results

In comparing the above values with those obtained on the phenolic-nylon

The permeability on both the virgin and charred materials was

Apparatus and Procedure

The apparatus employed for both virgin and charred material is

P = mean pressure in specimen

Q = flow rate through specimen, defined at mean pressure

AP = pressure drop through specimen

This admittance value is applicable to the combined Poiseuille (viscous)

Permeating gases of helium and nitrogen were used in this investiga-

Data and Results

Charred material. - For the degraded material, the admittance was

Q z flow of gas through the sample (corrected for Knudsen and

AP = pressure drop across the specimen

6 = exponent which is 0. 5 for turbulent and 1.0 for laminar flow

Using the data shown in Table 9, an approximate value of 6 can be

« « « «- o o» t- <o u> * COM-H 22 £5 K !£

4—?£) V mathematical solution o

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