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OTS PB 171423 DMIC Report 154
May 25, 1961
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EVOLUTION OF ULTRAHIGH-STRENGTH,
HARDENABLE STEELS FOR
SOLID-PROPELLANT ROCKET-MOTOR CASES
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The Defense Metals Information Center was established at
Battelle Memorial Institute at the request of the Office of the
Director of Defense Research and Engineering to provide Govern-
ment contractors and their suppliers technical assistance and
information on titanium, beryllium, magnesium, refractorymetals,
high-strength alleys for high-temperature service, corrosion-and
oxidation-resistant coatings, and thermal-protection systems. Its
functions, under the direction of the Office of the Secretary of
Defense, are as follows:
EVOLUTION OF ULTRAHIGH-STRENGTH,
HARDENABLE STEELS FOR
SOLID-PROPELLANT ROCKET-MOTOR CASES
by
to
Page
SUMMARY i
INTRODUCTION 3
General Comments 3
Low-Alloy Hardenable Steels 9
Chromium-Molybdenum Steels 11
Chromium-Nickel-Molybdenum Steels 14
5Cr-Mo-V Steels 19
REFERENCES 37
EVOLUTION OF ULTRAHIGH-STRENGTH,
HARDENABLE STEELS FOR
SOLID-PROPELLANT ROCKET-MOTOR CASES
SUMMARY
The information in this report was obtained from the Defense Metals
Information Center files at Battelle Memorial Institute and from other pub-
lished literature.
3
INTRODUCTION
General Comments
The development of ever higher strength in steels has long been the
goal of much research in ferrous metallurgy. Through the years, espe-
cially because of the persistent demands of the aircraft and missile indus-
tries, the strength level of steel has been raised progressively. Currently,
for the larger solid-propellant rocket-motor cases, steels with strength-
to-weight ratios in the order of 1,000,000 are desired (i.e., some 280,000-
psi tensile strength). The primary means of increasing strength in steel
has been to increase the alloy content and to lower the tempering tempera-
ture after quenching.
Most of the steels which are being used, or are being investigated
for use, in present-day missiles can be divided into two major groups: the
low-alloy engineering steels and the Cr-Mo-V hot-work die steels
(H-ll and H-13 types). The low-alloy engineering steels can be further
subdivided into chromium-molybdenum (AISI 4100 series) and chromium-
nickel-molybdenum (AISI 4300 series) types. Figure 1 shows a classifica-
tion of typical steels in ';he three families. At the top of each list in the
figure is a typical standard AISI steel in the family, while a number of
proprietary steels and modifications are listed below. *
5Cr-Mo-V
Cr-Mo Cr-Ni-Mo Hot-Work Die Steels
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between the flow (yield) and fracture (ultimate) stresses is small and,
hence, the ductility and resistance to brittle failure are low. Tempering
serves to increase the toughness and ductility of the steel, although
strength and hardness are sacrificed. Generally, the higher the temper-
ing temperature, the greater will be the ductility but the lower will be the
strength and hardness of a given steel.
When a steel part is cooled very rapidly after it has been austeni-
tized, as it is in quenching, residual stresses of considerable magnitude
are introduced, even in the absence of a transformation reaction. This
condition arises because, during very rapid cooling, the surface cools
most rapidly and a large temperature differential exists between the sur-
face and the center of the part. In addition, a volume expansion is
associated with the formation of martensite. This expansion introduces
additional stresses into the part. These residual stresses arising from
quenching and from transformation lower the external load that a part can
carry. Therefore, an important function of tempering is to relieve these
internal stresses. ,
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Tempering Temperature, F, for I Hr A-37551
Chromium-Molybdenum Steels
Steels in this category that are used or that are under consideration
for use in the missile industry for solid-propellant rocket-motor cases are
listed in Table 2; chemical compositions are included. The first steel in
this list is AISI 4130, which can be considered to be the base steel from
which the others evolved. When working stresses in welded aircraft parts
reached a point where plain-carbon steels were no longer satisfactory,
AISI 4130, a mildly air-hardening steel, was developed to meet the new
requirements. Increased hardenability over that of its plain-carbon
counterpart is obtained from the chromium and molybdenum additions.
This steel is characterized by excellent strength-to-weight ratio and
outstanding weldability, and has been a most important material in
aircraft structural assemblies. In addition, it has been used for other
engineering construction involving high stresses, particularly where ex-
tensive welding and medium hardenability are required.
(a) This is an experimental steel. The analysis shown is a typical analysis listed in the Universal Cyclops
brochure on UCX-2.
The wide use of this material in the aircraft industry and the re-
sultant familiarity with its characteristics made AISI 4130 steel a natural
early selection for use in high-strength rocket-motor cases. The other,
less familiar, chromium-molybdenum steels listed in Table 2, with the
exception of 17-22-AS, were evolved later, specifically for use in the
rocket and missile industry. The notable differences between the com-
position of AISI 4130 and thdse of the special steels are the higher carbon
and silicon contents in the latter and the addition of vanadium or, in UCX-2,
both vanadium and cobalt to the modified alloys. The higher contents of
carbon, chromium, and molybdenum increase the strength and the harden-
ability attainable on quenching, while the additions of silicon and cobalt
serve primarily to retard softening on tempering. Chromium, molybde-
num, and vanadium also contribute to resistance to softening on tempering,
but they are particularly effective at high tempering temperatures where
the formation of alloy carbides results in secondary hardening. Vanadium
is also effective in maintaining a fine grain size in the steel. These are the
advantages which these special steels offer over AISI 4130. They are
shown in Figure 5 which illustrates the strengths obtained and the retarding
of softening and weakening on tempering observed in the steels listed in
Table 2 (with AISI 4140 omitted).
300 400 500 600 700 800 900 lOOO 1100 1200 1300
Tempering Temperature, F A-3TSS2
Chromium-Nickel-Molybdenum Steels
The first steel developed in this group was AISI 4340. It was de-
signed for applications requiring higher strength or where heavier sections
are to be hardened throughout than would be feasible with AISI 4130. The
increased strength of this steel arises largely from increased carbon con-
tent, while increased hardenability stems from increases in manganese
and molybdenum and from the addition of nickel. This steel, too, has been
used for many years in the aircraft industry in landing gears and other
critical parts. At present, it is being used for parts heat treated to tensile
strengths up to 280,000 psi(13^ 14). Because of its widespread use and
industry's familiarity with this steel, it has become the standard high-
strength steel. The properties of AISI 4340 are used as a standard of com-
parison for other low-alloy hardenable steels during their development or
as a criterion for materials selection.
Of the steels in this group, AMS 6434(15) has been used more widely
than any other for fabrication of solid-propellant rocket-motor cases. This
steel is AISI 4340 with lower carbon for better weldability, with the molyb-
denum increased to compensate for the loss in hardenability caused by the
lower carbon content, and with vanadium added as a grain refiner. It is
used at heat-treated yield-strength levels of 185,000 to 210,000 psi. Re-
sistance to crack-propagation drops noticeably at higher strength levels.
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The other three steels in this group were developed specifically for
the aircraft industry for parts which require a combination of high strength
and toughness, such as landing gears. All three have been in existence for
a number of years. HY-Tuf was patented in 1948, while USS Strux and
300-M were introduced in 1952 and 1953, respectively.
AMS 6434 was developed from AISI 4340 by lowering the carbon con-
tent, increasing the molybdenum, and adding a small percentage of vana-
dium. As a result of these modifications, this steel shows better Charpy
impact values than does AISI 4340, both at 230,000- and at 250,000-psi
tensile strength. The same result is accomplished in Ladish D-6-A by
increasing the manganese and molybdenum and adding a small amount of
vanadium.
yield strength and ductility. Also, silicon shifts the so-called 500 F em-
brittlementj or tempered martensite brittleness, to higher tempering tem-
peratures. As a result, comparatively good notch toughness is obtained in
high-silicon steels tempered in the range from 400 to 600 F. Both 300-M
andHY-Tuf take advantage of these unique properties imparted by silicon.
5Cr-Mo-V Steels
The SCr-Mo-V steels have been used for many years for tools re-
quiring high strength and toughness at elevated temperatures. For about
25 years, a group of proprietary steels has been used in dies and fixtures
that commonly experience temperatures near 1000 F. These steels are
known as "hot-work tool steels", "hot-work die steels", or sometimes just
"die steels". Consideration of these steels for missile requirements is
based to a large extent on their comparatively high strength and high re-
sistance to softening at service temperatures from room temperature to
around 1000 F. Also, they have creep and stres s-rupture values compar-
able to those of superalloys at 1000 F. Up to 1200 F, some of these steels
have the highest strength-to-weight ratio of any commercial structural
metal, because they can be heat treated to tensile strengths of from 260,000
to 300,000 psi at high tempering temperatures. (2 !) Another feature of
these steels is greater stress relief, accomplished by tempering at rela-
tively high temperatures, as compared with the low-alloy engineering steels.
This is especially important in welded components, such as rocket-motor
cases.
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Tempering Temperature, F A-37556
Because of this slow cooling, the residual stresses that would result from
quenching are avoided.
Typical heat treatments for some of the steels in this class will be
shown later in the section of this report on heat treatment.
drawing large components, such as heads for rocket cases, from sheet
stock, the material frequently is given a special annealing treatment before
being shaped. The object is to create the most favorable type of micro-
structure in the steel for the forming operation.
The chromium hot-work die steels can be formed, drawn, and spun
with little more difficulty than the more familiar low-alloy hardenable
steels. (25,26) Properly annealed material and correctly spaced inter-
stage annealing are very important with these steels. When chromium
hot-work die steels are very heavily cold worked, as in severe deep-
drawing operations, it is advisable to stress relieve immediately to avoid
shattering on rough handling. Temperatures of the order of 7 50 to 925 F
are frequently used for this operation. Stress relieving should be done
soon after grinding, as well as prior to such operations as thread rolling,
shot peening, and plating. The process, or interstage, anneal may be
carried out at 1450 F followed by air cooling. An illustrative full-annealing
schedule comprises preheating to 1200 F, raising the temperature to
1650 F, and furnace cooling to 850 F followed by air cooling to room
temperature.
The parts should be thoroughly cleaned and free from rust, scale,
or oil bSfore heat treatment. Cleaning and descaling are preferably done
by mechanical means, such as sand, grit, or vapor blasting. Scale also
may be removed by anodic pickling. If the latter procedure is used, the
current should be on prior to and all during the immersion of the work in
the electrolyte. Acid pickling and cathodic pickling invite embrittlement
from absorption of hydrogen, and should be avoided.
The two welding processes that are used more widely than any others
for solid-propellant rocket-motor case fabrication are the inert-gas
tungsten-arc process and the submerged-arc process. The submerged-
arc process has the following limitations as compared with the inert-gas
tungsten-arc process: (1) chemical composition is more difficult to con-
trol; (2) the minimum plate thickness that can be welded with reasonable
success is about 1/8 inch; and (3) the lack of visibility of the submerged-
arc process makes it mandatory that weld-seal tracking be good. (**) The
25
Preheat and postheat are used for two reasons — to help reduce or
prevent weld-metal cracking and to produce an as-deposited weld-metal
micro structure of maximum ductility for ease of handling. Most rocket-
motor-case welding fixtures are fitted with heaters to provide the preheat
and postheat. For this reason, the postheat is usually the same tempera-
ture as the preheat. There is wide disagreement over the optimum preheat
and postheat temperatures for welding the various steels used for cases.
In general, the lowest preheat and postheat temperatures that can be used
satisfactorily to produce a structure of maximum ductility are employed.
Heat Treating
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Hydrogen Embrittlement
The following observations have been made in the brief period that
ausforming has been under systematic investigation. (^5) strength levels
are generally a function of the percentage of deformation, the temperature
of deformation, and the degree of subsequent tempering. A critical degree
of deformation is required before any significant increase in strength is
obtained; after this level is reached, strengths increase uniformly with in-
creasing amounts of deformation. With high degrees of deformation, the
yield and ultimate strengths become approximately equal.
Vacuum Melting
All the types of steel discussed in this report have been produced
experimentally, or are now being produced commercially, by vacuum
melting.
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REFERENCES
(2) Metals Handbook, 1948 Edition, Am. Soc. Metals, Cleveland, Ohio,
p 457.
(11) "U.S.S. Air Steel X-200, An Air Hardening Steel for Solid Propellant
Missile Motor Cases", United States Steel, 2nd Revision (June, 1959).
(15) March, J. I.. , "AMS 6434 (Modified) Steel Sheet Material Character-
istics and Heat Treatment", American Car and Foundry Division,
ACF Industries, Inc. , Major Report 458 (June 18, 1959).
(17) "U. S. S. Strux, An Alloy for Forged or Machined Aircraft and Missile
Parts", United States Steel Corp. , Pittsburgh, Pa. (September, 1958).
(23) Ruff, P. E. , "Hot Work Tool Steel for Aircraft", Metal Progress,
75 (3), March 1959, 103, and 75 (4), 97 (April, 1959J: """^
HJH:ARE:AMH/ims:pa:jvo
W*»**"
Columbus 1, Ohio
Copies of the technical reports listed below may be obtained from DMIC at no cost by Government agencies, and by
Government contractors, subcontractors, and their suppliers. Others may obtain copies from the Office of Technical Services,
Department of Commerce, Washingington 25, D. C. See PB numbers and prices in parentheses.
DMIC
Report Number Title
46D Department of Defense Titanium Sheet-Rolling Program - Uniform Testing Procedure for Sheet Materiali,
September 12, 195» (PB 121649 $1. 26)
46E Department of Defense Titanium Sheet-Rolling Program - Thermal Stability of the Titanium Sheet-Rolling-
Program Alloys, November 25, 1958 (PB 151061 $1.25)
46F Department of Defense Titanium Sheet-Rolling Program Status Report No. 4, March 20, 1959 (PB 151066 $2.25)
46G Department of Defense Titanium Sheet-Rolling Program - Time-Temperature-Transformation Diagrams of
the Titanium Sheet-Rolling Program Alloys, October 19, 1969 (PB 161075 J2.25)
46H Department of Defense Sheet-Rolling Program, Status Report No. 5, June 1, 1360 (PB 151087 J2.00)
461 S.atistical Analysis of Tensile Properties of Heat-Treated Ti-4Al-3Mo-lV Sheet, September 16, 1960
(PB 151096 $1.25)
106 Beryllium for Structural Applications, August 15, 1958 (PB 121648 $3.00)
107 Tensile Properties of Titanium Alloys at Low Temperature. January 15, 1959 (PB 161062 $1. 25)
lud Welding and Brazing of Molybdenum, March 1, 1969 (PB 161063 $1. 25)
109 Coatings for Protecting Molybdenum From Oxidation at Elevated Temperature, March 6, 1959 (PB 151064
$1.26)
HO The All-Beta Titanium Alloy (Ti-13V-llCr-3Al). April 17, 1959 (PB 151066 $3.00)
111 The Physical Metallurgy of Precipitation-Hardenable Stainless Steels, April 20, 1959 (PB 151067 $2.00)
112 Physical and Mechanical Properties of Nine Commercial Precipitation-Hardenable Stainless Steels,
May 1, 1959 (PB 151068 $3.25)
113 Properties of Certain Cold-Rolled Austenitic Stainless Sheet Steels. May 15, 1959 (PB 151069 $1.75)
114 Ductile-BnttleTransition in the Refractory Metals, June 25, 1959 (PB 151070 $2.00)
US The Fabrication of Tungsten, August 14, 1959 (PB 151071 $1. 75)
116R Design Information on 5Cr-Mo-V Alloy Steels (H-ll and 5Cr-Mo-V Aircraft Steel) for Aircraft and Missiles
(Revised), September 30, 1960 (PB 161072-R $1. 50)
117 Titanium Alloys for High-Temperature Use Strengthened by Fibers or Dispersed Particles, August 31 1959
(PB 151073 $2.00) .
118 Welding of High-Strength Steels for Aircraft and Missile Applications, October 12, 1959 (PB 151074 $2.25)
119 Heat Treatment of High-Strength Steels for Aircraft Applications, November 27, 1969 (PB 151076 $2.50)
120 A Review of Certain Ferrous Castings Applications in Aircraft and Missiles, December 18, 1959 (PB 161077
$1.50)
121 Methods for Conducting Short-Time Tensile, Creep, and Creep-Rupture Tests Under Conditions of Rapid
Heating, December 20, 1959 (PB 151078 $1.25)
122 The Welding of Titanium and Titanium Alloys, December 31, 1959 (PB 151079 $1. 75)
123 Oxidation Behavior and Protective Coatings for Columbium and Columbium-Base Alloys, January 15 1960
(PB 151080 $2.25) .
124 Current Tests for Evaluating Fracture Toughness of Sheet Metals at High Strength Levels, January 28 1960
(PB 151081 $2.00) '
Physical and Mechanical Properties of Columbium and Columbium-Base Alloys, February 22 1960
(PB 151U82 $1.75)
126 Structural Damage in Thermally Cycled Rene 41 and Astroloy Sheet Materials, February 29 1960
(PB 151083 $0.75) '
127 Physical and Mechanical Properties of Tungsten and Tungsten-Base Alloys, March 15, 1960 (PB 151084)
128 A Summary of Comparative Properties of Air-Melted and Vacuum-Melted Steels and Superalloys,
March 28, 1960 (PB 151085 $2. 75)
129 Physical Properties of Some Nickel-Base Alloys, May 20, 1960 (PB 151086 $2. 75)
130 Selected Short-Time Tensile and Creep Data Obtained Under Conditions of Rapid Heating June 17 1960
(PB 161088 $2.25)
131 New Developments in the Welding of Metals. June 24, 1960 (PB 151089 $1.25)
132 Design Information on Nickel-Base Alloys for Aircraft and Missiles, July 20, 1960 (PB 151090 $3.00)
133 Tantalum and Tantalum AUoys, July 26, 1960 (PB 151091 $5.00)
134 Strain Aging of Refractory Metals, August 12, 1960 (PB 151092 $1. 75)
135 Design Information on PH 15-7 Mo Stainless Steel for Aircraft and Missiles, August 22, 1960 (PB 151093 $1.25)
DMIC
Report Number Title
136A The Effects of Alloying Elements in Titanium, Volume A. Constitution, September 16.1960(PB 151094 $3. 50)
137
Design Information on 17-7 PH Stainless Steels for Aircraft and Missiles, September23, 1960{PB 151096$!. 00)
138 Availability and Mechanical Properties of High-Strength Steei Extrusions, October 26, 1960 (PB 151097 $1. 75)
139 Melting and Casting of the Refractory Metals Molybdenum, Columbium, Tantalum, and Tungsten,
November 18, 1960 (PB 151098 $1.00)
140
Physical and Mechanical Properties of Commercial Molybdenum-Base Alloys, November 30, 1960
141 Titanium-AUoy Forgings, December 19, 1960 (PB 1SH00 $2.25)
142
Environmental Factors Influencing Metals Applications in Space Vehicles, December 27, ia6ü(PB 151101 $1.25)
143 High-Strength-Steel Forgings, January 5, 1961
144
Stress-Corrosion Cracking - A Nontechnical Introduction to the Problem, January 6, 1961 (PB 151103 $0.75)
145
Design Information on Titanium Alloys for Aircraft and Missiles, January 10, 1961
148
Manual for Beryllium Prospectors, January 18, 1961
147 The Factors Influencing the i-racture Characteristics of High-Strength Steel, February 6, 1961
148
Review of Current Data on the Tensile Properties of Metals at Very Low Temperatures, February 14. 1961
149
Brazing for High Temperature Service. February 21, 1961
159 A
Review of Bending Methods for Stainless Steel Tubing, March 2, 1961
151 Environmental and Metallurgical Factors of Stress-Corrosion Cracking in High-Strength Steels, April 14, 1961
152 Binary and Ternary Phase Diagrams of Columbium, Molybdenum, Tantalum, and Tungsten, April 28, 1961
153
Physical Metallurgy of Nickel-Base Superalloys, May 5, 1961,
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