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MATERIALS PROBLEMS ENGOUNTERED

IN LIQUID PROPELLANT ROCKET ENGINES

DONALD E. RODA

Rocketdyhe
Div. of North American Aviation, Inc.

For presentation a t the

SAE ANNUAL MEETING
Sheraton-Cadillac & S t a t l e r Hotels
D e t r o i t , Michigan
January 12-16, 1959

Written discussion of this paper will be accepted by SAE until Feb.16, 1959.
Three double-spaced copies are appreciated.

SOCIETY of AUTOMOTIVE ENGINEERS, Inc.,485 Lexington Avenue,New York 17, N.Y.

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MATERIALS PROBLEMS ENCOUNTERED

IN LIQUID PROPELLANT ROCKET ENGINES

Covering the temperature range of -300oF to +5000oF the materials problems

encountered in liquid propellant rocket engines are great and different from those
encountered in other types of engines. Fortunately, for us, it is possible to re-
generatively cool those parts of the engine that are subject to temperatures over
1500oF.

The design, fabrication, and testing of liquid propellant rocket engines

are fairly new to those outside the rocket industry. Therefore, I would like to
cover this subject in a general way, in addition to dealing with some of the specific
material requirements. It is quite possible that you might be called upon to build
similar engines, or at least to produce components that will be used in these
engines, in which case a general understanding of the engines, the need for high
quality materials, and good reliability will be worthwhile.

In order to present the whole picture, the paper will be broken into
three parts: 1. An explanation of a typical liquid propellant rocket engine,
2. The testing and use of these engines, and 3. A broad picture of the material re-
quirements and material problems encountered with this typical rocket engine.

Typical Large Rocket Engine

Fig. 1 is a cutaway sketch of a typical large liquid propellant rocket

engine. The oxidizer (usually liquid oxygen) enters the engine through the ducting
on the lower left hand side of the sketch. An expansion bellows is required in
this line. The LOX passes through the inducer, which is used to prevent cavitation
in this low boiling point liquid, through the impeller, and out of the pump housing
into the dome chamber of the injector or burner. Likewise the fuel, which can be
RP1 or kerosene, enters through the duct on the upper left hand side of the engine,
through the pump to the thrust chamber. This is a double wall chamber and the fuel
is circulated through the chamber to keep it cool before entering the fuel passages
in the injector. The main propellant valves are located in the oxidizer and fuel
lines, just ahead of the injector, and are of the rotating gate or butterfly type
that rotate through and seal on a thermoplastic lip seal (usually made of Kel-F for
both fuel and oxidizer rather than a rubber or elastomeric material).

The propellant pumps are driven by a turbine through a gear box and gear
train. This allows the turbine to operate at higher speed and reduces its size.
In turn the turbine is driven by the products of combustion from a gas generator
at the upper left hand side of the engine. After passing through the turbine and
accomplishing its work the combustion products are expelled out the exhaust pipe
located above the turbine. The sketch shows the gas generator connected to the
main fuel and oxidizer lines as the source of its propellants in boot strap opera-
tion. For starting operation pressurized propellant start tanks are often required.

Pressurization of the main propellant tanks to a fairly high pressure to

drive the propellants into the injector and thrust chamber instead of pumping is
an alternate system; however, it is not as efficient from a weight standpoint for a
complete engine rocket system as one using a turbopurap for propellant feed.
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The liquid propellants meet in the combustion chamber across the face of
the injector to produce a tremendous volume of gas at a temperature over 5OOOoF.
The combustion is regulated to produce sonic velocity of the gases at the throat
of the DeLaval nozzle and supersonic velocity as the product of combustion expands
out of the cone of the chamber according to laws of conservation of momentum, mass
and energy.

Components not shown in the sketch of the typical large rocket engine
are: the hydraulic and pneumatic systems to operate valves, the gimbal bearing on
which the thrust chamber can be rotated in any direction for steering the rocket,
the electrical system to receive the guidance signals and for sequential operations,
the thrust mount or frame to transmit the thrust from the engine to the rocket as-
sembly and provide mounting structure for some of the components, igniters to light
off the gas generator and main thrust chamber and other items which combine to make
the complete large rocket engine. A picture of a completed Thor IREM liquid pro-
pellant rocket engine is shown in Fig. 2 less the turbine exhaust pipe.

Use and Testing of Large Rocket Engines

. Contrary to popular belief, the operation of a large liquid propellant

rocket engine is not a one-shot performance. The individual components are test
fired separately. Engines are assembled from proven components and again test
fired and calibrated. After insulation of the engine into the rocket the overall
system may again be static fired and the thrust measured.

Fig. 3 shows a blade valve being installed on a turbopump and gas genera-
tor assembly in the components hot firing test area with the large propellant lines
feeding down to the pump inlet. Considerable instrumentation is connected for mea-
suring temperatures, pressures, flow, speed, etc.

An overall view of a components test laboratory is seen in Fig. 4. All

personnel are located inside the building while the test firing of a gas generator
is going on. Several test cells are located along the back of the building and the
location of test facilities in pockets in rugged terrain, remote from populated
areas is readily seen. The large overhead tanks are used to store and recirculate
propellants. At ground level four pits are used for component testing and three
static test stands permit complete rocket engine cold calibration pre-acceptance
tests.

The test firing of a large liquid propellant rocket engine is clearly

shown in Fig. 5. The test stands are made of structural steel and are well anchored
into the ground. Capable of withstanding thrusts of one million pounds, these
stands enable engineers to measure thrust, temperature, pressure, valve operation
and other performance characteristics from nearby recording centers. Large pro--
pellant tanks are located high above the stand, similar to a rocket installation.
Platforms are provided for mounting and connecting the engine. A water-cooled
flame bucket is used to turn the supersonic rocket flames 90o out away from the
test stand. The firing is controlled from a block house not far away where controls
and recording instruments are located.

A cluster of 3 large rocket engines are shown projecting out of the tail of
a U.S. Air Force Atlas ballistic missile in Fig. 6. (An added third engine will give
the Atlas ballistic missile intercontinental range of more than 6,000 miles. The new
sustainer is in the center of the thrust section; the booster engines on either side
are the same as those that powered earlier Atlas test flights. Angled pipe above the
sustainer engine is the turbopump exhaust.) Here the complete rocket and engine as-
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semblies are being prepared for hold down t e s t operation and t e s t f i r i n g a t the
Missile S t a t i c Test S i t e , Edwards Air Force Base, California. Increased perform-
ance i s obtained through the use of a c l u s t e r of a l l 3 engines to boost the rocket
t o high a l t i t u d e and then a remaining single engine to further increase the a c -
celeration and sustain the f l i g h t .

F i n a l l y , a f t e r hours of painstaking work and hazardous t e s t i n g , the

rockets are f i r e d and released a t the t e s t center in Cape Canaveral, F l o r i d a .
Fig. 7 shows a liquid propellant U.S. Air Force Thor intermediate range b a l l i s t i c
missile leaving the launching s i t e . (The l i q u i d - p r o p e l l a n t power supplied by the
Rocketdyne engine system includes two small vernier engines mounted on opposite
sides of the missile a f t section t o provide s t a b i l i t y . ) From here on the auto-
matic guidance systems and ground tracking s t a t i o n s take over. The Thor missile
was used as the f i r s t stage or booster on the Air Force's lunar probe mission
October 1 1 , 1958, to boost a 50-ton vehicle 90 miles i n t o space before the second
and t h i r d stages took over t o accelerate the Pioneer space probe vehicle t o a
speed of s i x and one-half miles a second and obtain a distance of almost 80,000
miles above the E a r t h ' s surface before the pull of gravity turned the Pioneer
back to Earth.

MATERIALS PROBLEMS

What are the materials problems encountered i n a liquid propellant

rocket engine? Are they peculiar t o rocket engines or are they similar t o thoee-
of other types of engines and s t r u c t u r e s ? The thought immediately comes to mind
about the use of titanium, beryllium, and other exotic l i g h t weight, high strength
materials; and of molybdenum, tungsten, cermets, and refractory materials for high
temperature service. The material problems i n production processing and fabrica-
tion of these r e l a t i v e l y new members of the engineering materials family are well
founded.

Such are not the material problems of the present liquid propellant rocket
engines. They are much more closely related to i n t e r n a l combustion and j e t engines,
except t h a t the loads are higher, the operating l i f e i s s h o r t e r , and there i s the
problem of handling low temperature f l u i d s l i k e liquid oxygen or l i q u i d nitrogen.

Some of the t y p i c a l materials problems with large l i q u i d propellant

rocket engines a r e :

Thermal Expansion, or more accurately d i f f e r e n t i a l thermal expansion, i s

a problem such as i n the b o l t s t h a t hold the volute of the l i q u i d oxygen pump c a s t -
ing together and the vanes in place. High strength b o l t s are required and the bolt
diameter i s limited by the vane thickness. The greater contraction of the aluminum
a l l o y casting shrinks i t away from the b o l t s (which are approximately 3" long),
leaving the b o l t s loose or completely without i t s torqued p r e - s t r e s s load. Good
low temperature strength and toughness are required along with a high thermal co-
e f f i c i e n t of expansion i n these b o l t m a t e r i a l s . A-286 heat t r e a t e d t o ah ultimate
strength l e v e l of l45,000 psi with a coefficient of expansion of 8.3 as compared
to aluminum with 10.5 i s b e t t e r than heat t r e a t e d Iriconel X with an ultimate
strength of 175,000 psi and a coefficient of 5.7 i f there i s an appreciable length
of material involved.

Low Temperature Mechanical Properties are a r e l a t e d problem. Type 410

and 440C s t a i n l e s s s t e e l s were of i n t e r e s t because of t h e i r increased corrosion
resistance and high strength in the heat t r e a t e d condition. Parts made without
sharp corners or s t r e s s r a i s e r s and not subject to impact loads, such as the shaft
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for the gate of the main oxidizer (liquid oxygen) valve, have been successfully
operated with these materials. The martensitic materials in the heat treated
condition are subject to a low temperature transition from ductile to brittle
type of failure and the low temperature mechanical properties at -320OF (liquid
nitrogen testing temperature) had not been previously determined. In these cases
it was necessary to conduct our own tests to determine the low temperature mech-
anical properties.

Fig. 8 shows a large increase in ultimate and yield strengths from room
temperature, white area, to low temperature -320OF, black area, for the 400 series
stainless steels in the heat treated condition. Also, there is considerable re-
duction in elongation at low temperature, black area, with about 7% remaining for
4lO steel and 2% for the harder, stronger grade of 44OC steel. These properties
are required for efficient design and accurate stress analyses.

Figs. 9 and 10 show the care that must be exercised in preparation of

the test specimens and button grips to eliminate stress riser and obtain accurate
results. Fig. 11 is a photograph of the special extensometer required for opera-
tion in liquid nitrogen and Fig. 12 shows a low temperature test in progress with
the container of liquid nitrogen raised up around the test sample and the lower
portion of the extensometer.

Fatigue of Gear Teeth is a good example of the type of material problems

that are brought to attention for solution through failure analyses. Fig. 13 is
of ah intermediate gear with two teeth missing after 1700 seconds of test opera-
tion. While a close-up of the fractured tooth area reveals the typical bench
marks of a fatigue failure, Fig. l4, that is more typical of many hours or months
of operation at ndrmal loads. The need for high quality gears is evident.

The gears are made of SAE 9310 steel to AMS Specification 6260E, car-
burized to a final case depth of .025" to .035" and hardened to Rockwell "C" 60
-minimum.

The failure analysis showed unsatisfactory heat treated structure, non-

uniform case depth and inaccurate tooth contour. Gear failures have been com-
pletely eliminated through tightening quality standards and inspection require-
ments. A special carburizing and heat treating specification was prepared with
very close processing requirements, detailed procedures, and more rigorous in-
spection requirements. The vendors were contacted to be certain that they under-
stood the problem and the need for high quality and several hours of satisfactory
test operation. Apart from the metallurgical requirements, more accurate gears
were obtained dimensibnally. Steps were taken to verify alignment of the shafts
in the gear box and accurate center distances. All of these things combined to
produce gears that could stand the rigors of test operation and improve the re-
liability of the engines.

Tens-50 Aluminum Castings comprise a large part of the turbopump and are
used for other parts of the rocket engine. Originally 356-T6 aluminum castings
were used for the oxidizer and fuel volutes, the impeller and the gear box castings.
Increased power requirements and upgrading of turbopumps and engines put increasing
loads on the pump parts and castings.

The strength and quality of the castings were progressively increased

through the use Of sodium modified 356-T6, the high purity 355-T6 and 356-T6, and
finally through the use of a new alloy developed at the Inglewood Plant of N.A.A.
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known as Tens-50 (50,000 psi ultimate tensile strength) for which a patent has been
applied for on this alloy and information concerning it may be obtained from NAVAN
Products, Inc., 900. N. Sepulveda Blvd., El Segundo, Calif.

In addition, a special Rocketdyne casting survey team was formed com-

posed of Engineering, Quality Control, and Purchasing to visit the foundries in
the Los Angeles area and others located all the way to the East Coast to explain
our requirements and to evaluate the foundries' desire and ability to produce uni-
form high strength, high quality castings. The strength of the castings have been
more than doubled and adequate ductility maintained. Through a vigorous Quality
Control follow-up program the mechanical properties of all lots of production
castings are determined and the quality held at the high level needed for these
critical parts.

Compatibility is one of the more recent and interesting of the liquid

propellant rocket engine material requirements. With the introduction of some of
the high energy and storable propellants, problems in corrosion resistance and
compatibility of metals and plastics with these chemically active liquids have
arisen. A storable oxidizer can be described as an oxidizer that is liquid near
or at ambient temperatures and pressures. For example, nitrogen tetroxide (NT0)
has a freezing point of +13F and a boiling point of +68F and is a powerful
oxidizer. In the presence of water it forms both nitric and nitrous acid.
Fig. 15 shows the operating mechanism of the main propellant oxidizer valve after
less than two hours of operation with NT0. The cadmium plating of the steel parts
has been almost completely removed and the steel is heavily rusted, while in the
valve itself, Fig. 16, the NT0 has removed the anodized coating from the 75ST
aluminum gate, softened the Kel-F lip seal so that part of it broke away and is
missing, and rusted the lock ring for the lip seal retainer ring. The breaking
of the lock ring into three pieces upon removal from the valve also indicated that
it had been subjected to hydrogen embrittlement.

The problems of compatibility can be solved through the proper selection

of materials, plating and protective coatings for materials. They vary to a great
extent with the parts. The material and service requirements for a tank are con-
siderably different from those of shaft or valve. One might have continuous ex-
posure of both vapors and liquids while the other might have intermittent exposure
to either liquid or gas.

To say that all of the compatibility problems have been solved would be
a gross overstatement. In fact, protection of materials for adequate corrosion
resistance and long time storage of present rocket engines with present propellants
and compatibility of materials with new propellants will be one of the biggest and
continuing areas of materials problems in rocket engines.

There are many other areas of materials problems, too numerous for com-
plete coverage; perhaps a few words about each would be of interest. In the field
of fabrication, welding and brazing in all their forms are used to a great extent
with considerable development work required for the particular part. An example
is the welding of cast Stellite 21 blades to 16-25-6 wheels for turbine wheels.
So many blades are required that there is not enough room for fir tree or mechani-
cal attachment. Fig. 17 shows an experimental first stage wheel with interlocking
shrouds on the tip of the blades. The short time elevated temperature properties
of metals and non-metals is of interest to the rocket engine industry as compared
to the one hundred to several thousand hour properties of interest to most other
industries.
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Several non-metallic materials are involved including hydraulic o i l for
operation of valves and gimbaling the engine. Extremely clean hydraulic o i l i s
required for s a t i s f a c t o r y operation of the servo valve mechanisms which provide
the tremendous multiplication of power i n small u n i t s t o transform the e l e c t r i c a l
impulses or electronic signals i n t o forces t h a t w i l l control the rocket engine.
A program for the establishment of standards for the amount and size of d i r t
p a r t i c l e s in hydraulic o i l i s in progress.

The c h a r a c t e r i s t i c s of o i l s for lubricating and cooling the gear box i s

of importance both a t sea l e v e l or ambient pressure and a t high a l t i t u d e s where
engines and components must operate i n almost a complete vacuum unless they are
pressurized. The MIL-L-6068 o i l t h a t i s used for l u b r i c a t i o n foams a t high a l t i -
tude unless an anti-foam agent i s added or the gear box i s pressurized. Dry film
lubricants such as the moly sulfide coatings are used on some components of the
engine and i t has been found through a l t i t u d e chamber t e s t s t h a t a high vacuum or
lack of moisture and oxygen a t high a l t i t u d e s increases the coefficient of f r i c t i o n
of these materials to a great extent.

Structural or reinforced thermosetting p l a s t i c s are used for some a p p l i -

c a t i o n s , composed of glass roving and epoxy r e s i n , high strength, combined with
good elevated temperature r e s i s t a n c e , and good bonding are the properties desired
of these m a t e r i a l s .

Thermoplastics are used f o r both dynamic and s t a t i c s e a l s . Kel-F i s

used for both the oxidizer and fuel l i p s e a l s . This appears t o be the only
p l a s t i c type of material t h a t r e t a i n s some f l e x i b i l i t y a t -300OF or l i q u i d oxygen
temperatures. 0-rings and F l e x a t a t i c gaskets with s t a i n l e s s s t e e l rings and
asbestos f i l l e r material are used f o r s t a t i c seals i n flange-type j o i n t s . Design-
ing l i g h t weight j o i n t s and obtaining s a t i s f a c t o r y seals i s always a d i f f i c u l t pro-
blem.

Liquid propellant rocket engines are not a one-shot operating u n i t . They

are assembled out of components t h a t have been t e s t f i r e d many times. Calibration
i s required of many of the components. Careful, clean assembly i s required of the
components i n t o a finished engine t h a t i s t e s t fired several times t o e s t a b l i s h i t s
r e l i a b i l i t y , s t a r t i n g and stopping c h a r a c t e r i s t i c s , and ultimate t h r u s t when the
time comes for i t t o l i f t a s c i e n t i f i c vehicle or missile i n t o space.

All of the raw m a t e r i a l s , several of the individual p a r t s , and complete

assembled components are obtained from vendors. A large l i q u i d propellant rocket
engine produces about 50 times the t h r u s t of a j e t engine on a thrust-to-weight
b a s i s . Although the operating l i f e i s much shorter, the loads are much higher
and i t i s important for a l l of those who are making parts for these rocket engines
or who are thinking of building rocket engines t o r e a l i z e t h a t more s t r i n g e n t r e -
quirements are needed for the component parts than are required of j e t engine
p a r t s , and high q u a l i t y standards must be obtained.
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The room temperature mechanical properties are the white area in the bar
graph and the low temperature properties are the solid or black area. There
is considerable increase in both Ultimate and Yield strength with a corresponding
loss in ductility as indicated by elongation. Although the elongation of the
440C type steel is only a little over 1% in the high strength heat treated
condition at -320 F it must be remembered that it is only a little over 2% at
room temperature.
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Figs. 9 & 10 Test bars free of stress raiser in the reduced section test area
are shown in Pig. 9 and the use of button type grips to pull these extremely
hard materials without introducing bending loads or stress concentrations are
shown in Fig. 10.
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Figs. 11 & 12 An extensometer with long extension arms from the operating
mechanism are required for immersion with the test bar down into the con-
tainer of liquid nitrogen as shown in Fig. 11. A low temperature test is in
operation in Fig. 12 with liquid nitrogen in the container around the test
bar. The long extension arms from the cross heads of the testing machine are
used to eliminate bending loads in testing high strength steel test specimens.
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A close up of the missing gear tooth area in Pig. 13 reveals the tell-tale
beach marks of fatigue failure normally encountered only after many hours of
operation of conventional equipment.
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Corrosion of 4130 steel parts of the main oxidizer valve operating mechanism.
This valve was removed from an engine after 2 hours and 47 minutes of exposure to
one of the storable propellants, nitrogen tetroxide. Cadmium plating and black
oxide coating have offered no protection to the steel parts and they are severely
rusted, after the shaft seal failed and allowed the oxidizer to leak into actuating
mechanism chamber.
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The gate of the same main propellant oxidizer valve as discussed in Fig. 15
shows failure of the Kel-F lip seal through loss of tensile strength in NTO,
corrosion of the lip seal [Link] the anodized coating was eaten away from
the 75ST aluminum gate. The 321 stainless steel lip seal retainer ring was still
in good condition after the 2 hour and 47 minute exposure to nitrogen tetroxide,
storable oxidizer.
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