ASM Handbook, Volume 4E, Heat Treating of Nonferrous Alloys Copyright # 2016 ASM InternationalW

G.E. Totten and D.S. MacKenzie, editors All rights reserved

DOI: 10.31399/asm.hb.v04e.a0006256 www.asminternational.org

Heat Treating of Uranium and

Uranium Alloys*
Reaffirmed by Robert Hackenberg, Los Alamos National Laboratory

THE MAJOR APPLICATIONS of depleted and hydride formation; ready oxidation in air, Phase Changes. Chemically and metallurgi-
uranium (DU) and its alloys are those for which attack by hot water; and dissolution by acids. cally, DU is identical with natural uranium.
density is an important, if not an overriding, con- In addition, fine particles of uranium metal are Transformation from the alpha phase (ortho-
sideration (at 19.05 g/cm3, unalloyed depleted pyrophoric and can ignite spontaneously at room rhombic) to the beta phase (tetragonal) occurs
uranium is one of the densest of all elements). temperature. at 662
C (1224
F). The beta phase is stable
Among these applications are kinetic energy The metal uranium is obtained from uranium up to 773
C (1423
F), where it transforms
penetrators for military use, aircraft and missile hexafluoride (UF6) tailings from the uranium to the high-temperature gamma phase (body-
counter-weights, radiation shielding, gyrorotors, enrichment process that provides U-235 uranium centered cubic). The latter is stable to the melt-
high-energy physics calorimeters, and ballast. for the nuclear industry. In typical production of ing point, 1132
C (2070
F). The gamma
Dilute alloys containing 0.75 wt% Ti or 2 wt% depleted uranium, UF6 tailings are reduced to phase in unalloyed DU cannot be retained to
Mo are used in production of kinetic energy pene- uranium tetrafluoride (UF4), called “green salt,” room temperature by commercial quench rates.
trators (the largest single application of DU) which is further reduced to derby uranium metal Phase changes in DU and its alloys are
because superior mechanical properties can be by a thermite-type bomb reduction with magne- accompanied by significant changes in volume.
developed in these alloys, and their corrosion sium metal. Calcium metal has also been used Volumetric shrinkage from the high-tempera-
resistance can be improved, by heat treatment. to reduce UF4 to derby metal. Typical derby ture gamma phase to the low-temperature phase
Although most DU was originally produced in chemical analysis ranges (in ppm) are 5 to 50 is 1.8%. Changes in linear dimensions are influ-
cast form and used without heat treatment, cur- Cu, 8 to 40 Al, 30 to 150 Fe, 10 to 50 Ni, 10 enced by preferred orientation. For a random
rent material requirements usually call for heat to 100 Si, 1 to 10 Mg, 10 to 50 C, 15 to 40 O, orientation, linear shrinkage is 0.6%. Because
treated, wrought DU for property consistency. 8 to 40 N, and 4 to 18 H. Minor high-vapor- shrinkage cannot be predicted accurately, these
Ingot breakdown and primary fabrication pro- pressure contaminants can be removed by dimensional changes make it impossible to
cesses, such as forging, rolling, and extruding, volatilization during subsequent vacuum melting machine (DU) to final dimensions before heat
can be readily carried out between 550 and operations, while the other listed elemental con- treatment. In rough machining for heat treat-
640
C (1020 and 1180
F) or between 800 taminants remain. These impurities should be ment, an envelope at least 0.4 to 0.5 mm
and 900
C (1470 and 1650
F). The 650 to monitored and controlled to ensure expected met- (0.015 to 0.020 in.) thick should be allowed
780
C (1200 to 1435
F) range is avoided allurgical response to processing. Typical chemi- for final machining.
because cracking commonly occurs at these tem- cal and gas analyses for vacuum-induction-melted
peratures. Secondary fabrication processes such depleted uranium are shown in Table 1. In general,
as rolling, swaging, and straightening are com- hardness varies directly, and ductility varies Grain Size and Orientation Control
monly done between room temperature and inversely, with impurity content.
500
C (930
F). Following heat treatment, The grains of cast DU or of DU worked in the
machining to final dimensions can be carried gamma region are quite large, typically 2 to
out by most conventional cutting and grinding 3 mm (0.08 to 0.12 in.) in diameter. Large grain
techniques. This article focuses on the heat treat- Table 1 Typical chemical and gas analyses sizes are undesirable for material that is to be
ment of uranium alloys. Additional information for vacuum-induction-melted depleted worked because they result in rough machined
on processing, including heat treatment, is also uranium surfaces and variations in mechanical properties.
provided in Properties and Selection: Nonfer- Element Average analysis, ppm (by wt) On a macroscale, grain size can be refined con-
rous Alloys and Special-Purpose Materials, Carbon 180 siderably by multiple beta quenching. In work-
Volume 2 of ASM Handbook, 1990, and in the N2 15 pieces more than 25 mm (1 in.) thick, however,
Selected References at the end of this article. O2 40 refinement is limited to an outer layer of grains
Bulk H2 2 because the cooling rates at greater depths are
Aluminum 25
too low. Generally, the rim of fine-grained mate-
Metallurgical Characteristics Copper
Iron
15
85 rial is sufficiently thick to produce a smooth sur-
of Depleted Uranium Manganese 15 face after subsequent working.
Nickel 20 Beta treatment is also used as a heat treatment
Lead 4
In processing of uranium, several considera- Silicon 120 for DU worked in the high-alpha-temperature
tions must be addressed: hydrogen embrittlement range. Beta treatment consists of heating the

* Reaffirmed from: G.M. Ludtka and E.L. Bird, Heat Treating of Uranium and Uranium Alloys, Heat Treating, Vol 4, ASM Handbook, ASM International, 1991, p 928–938

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 668 / Heat Treating of Other Nonferrous Alloys

DU into the beta range, holding for a suitable temperature needed for uniform recrystalliza- of the cold work strain; cold working temp-
time, and cooling at a rapid rate. A common tion is lowered. For most formed parts made erature; and volume, size, and dispersion of
temperature range is 720 to 730
C(1330 to from relatively pure material, recrystallization inclusions. Cold or warm working of DU often
1350
F). The purpose of this heat treatment is will not occur below 400
C (750
F) with results in a banded or duplex structure; this per-
to eliminate the preferred orientation that devel- annealing times of up to 10 h. sists as a duplex grain size after recrystalliza-
ops during working. tion. The average grain size for material rolled
The final alpha grain size is insensitive to tem- to 50% reduction at 300
C (570
F) is illu-
perature within the beta range and to variations Cold Working strated in Fig. 2. This shows the effect of
in holding time. Times from 1 min to 1 h at tem- annealing temperature (annealing time, 1 h) on
peratures greater than 700
C (1290
F) have no Alpha uranium is slightly softer than steel materials of various purities. Grain size is
effect on final alpha grain size. Cooling rate, and is considered to be malleable and ductile. approximately 0.01 to 0.015 mm (0.0004 to
however, has a significant effect. Water- Alpha uranium is readily worked at room tem- 0.0006 in.) for impure uranium and as large as
quenched material has a significantly finer grain perature; however, directionality and texture 0.04 mm (0.0015 in.) for high-purity metal.
size, and the grains have scalloped edges, which persist because of a pronounced anisotropy. Table 4 presents typical mechanical proper-
are indicative of the massive transformation that Aside from the complication of directionality, ties of uranium in various conditions. These
occurs during rapid beta quenching. Air-cooled the tensile strength of uranium can be greatly data are not precise values and are intended
grains have more uniform boundaries. Extremely enhanced by cold working, as shown in Table 2; for use only as guidelines for selection of heat
low cooling rates, such as those obtained in a hardness also can be increased significantly, as treatments.
furnace-cool cycle, produce large alpha grains. shown in Table 3. The following heat treating procedure can be
Also, detrimental grain growth to as-cast grain followed to produce fine-grained material. It is
sizes can occur in wrought DU through an best to start with a relatively pure material that
extended alpha anneal. Annealing has very small amounts of inclusion-producing
High cooling rates such as those achieved by impurities. Following a hot breakdown of the
water quenching produce high residual stresses Annealing of cold-worked DU is similar to rolling ingot at 630
C (1165
F), rolling opera-
in beta-treated material. In thin sections, these that in other metals. The first stage is recovery, tions are performed at 300 to 400
C (570 to
residual stresses can produce appreciable plas- in which there is a slight decrease in hardness, a 750
F). After 40 to 60% warm work, the mate-
tic deformation in the alpha phase. This alpha small decrease in electrical resistivity, and a rial is given a short recrystallization anneal
phase can be recrystallized, and sometimes pronounced sharpening of x-ray line shape. (approximately 30 min per inch of thickness)
grain refined, by an anneal in the alpha range. Recovery is followed by recrystallization. The at 630
C (1165
F). The rolling stock is cooled
Alpha annealing after beta treatment will not variation of recrystallization temperature as a from the annealing temperature to below
produce recrystallization at the center of a thick function of cold work is shown in Fig. 1 for 400
C (750
F) and given further warm work.
section, because the center does not cool rap- an annealing time of 1½ h. Recrystallization This process is repeated as often as final stock
idly enough for sufficient straining of the lattice begins at 400
C (750
F) and is complete at thickness will allow.
to occur. 450
C (840
F) in material cold worked 90 to If the rolled stock is to be used in subsequent
When DU is water quenched from the beta 94%. Light cold working (approximately 4%) forming operations, the final rolling procedure
phase, high stresses develop due to the combi- causes recrystallization to begin at 525
C should leave 15 to 20% warm work in the plate.
nation of the radial temperature gradient and (975
F), but recrystallization is not complete Forming operations should be carried out warm
volume contraction during beta-to-alpha trans- after 1½ h at 600
C (1110
F). at temperatures not exceeding 375
C (705
F).
formation. These stresses are compressive at The grain size of cold-worked and annealed A final anneal at 630
C (1165
F) for 30 min
the surface and tensile at the center. The tensile DU depends on a variety of factors: annealing per inch of thickness (minimum, 6 to 8 min)
stresses are high enough to produce failure near time and temperature; amount and homogeneity will produce parts with a grain size of ASTM
the centerline. Large numbers of repetitive
quenches from the beta phase can produce
sponginess, cracks, or holes in the center sec- Table 2 Typical mechanical properties of depleted uranium as functions of amount of cold
tion of the workpiece. work
Grain growth is extremely sensitive to orien-
tation as well as to differences in metal purity, Ultimate tensile strength Tensile yield strength(a) Compressive yield strength

to prior deformation, and to heat treatments that Cold work, % MPa ksi MPa ksi MPa ksi Elongation(b), % Hardness(c), HV

affect the dispersions of contaminant second 0(d) 1060 154 375 54 405 58 15 294
phase. Those contaminants that are in solution 15 1140 165 525 76 500 72 17 352
tend to delay recrystallization and often result 25 1190 173 600 87 575 83 14 354
40 1280 186 660 96 605 87 13 359
in mixed, or incomplete, recrystallized struc- 55 1360 197 905 131 690 100 11 397
tures. Those elements having uranium com-
(a) At 0.2% offset. (b) In 50 mm (2 in.). (c) 1 kg load. (d) This material is highly directional and was not beta heat treated.
pounds that show limited solubility, thereby
existing as inclusions, do not delay recrystalli-
zation appreciably.
The amount of work that exists in uranium Table 3 Hardness data for cold-worked uranium rod
metal prior to heat treatment has an important
Hardness
effect on final grain size. A 1 to 2% strain in
HR15N HR30N HR30T HR45T HV(a)
uranium constitutes critical strain. Recrystalli-
Cold work, % Average Range(b) Average Range Average Range Average Range Average Range(c)
zation of material with this amount of strain
results in very large grains. Consequently, a 0 72 71–74 43 42–44 79 77–82 68 67–69 294 281–308
plate prepared for forming operations is pro- 15 73 71–74 46 42–49 81 79–82 72 69–73 352 335–366
25 75 74–76 47 43–49 81 79–83 73 71–74 354 348–361
duced with 10 to 15% warm work to ensure that 40 76 75–77 50 47–52 83 81–85 73 69–75 359 339–376
no areas of critical strain exist in the final 55 78 76–79 56 55–58 85 83–86 79 78–80 397 376–423
wrought product. As the amount of work in (a) 1 kg load. (b) Results of five indentations. (c) Results of eight indentations across the diametral cross section of the bar
the metal to be annealed is increased, the

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 Heat Treating of Uranium and Uranium Alloys / 669

6 to 10, depending on the amount of warm water quenched, and then given an alpha
rolling possible. Intermediate anneals at tem- anneal. Grain refining occurs because of the
peratures below the suggested 630
C presence of small levels of uranium-iron and
(1165
F) will help develop the finer grain size. uranium-silicon compounds. These compounds
Test specimens will be required to establish the are put into solution by the 740
C (1365
F)
times necessary at these lower temperatures to (or higher) beta heat treatment, kept in solution
effect complete recrystallization. by the water quench, and then precipitated
Alpha recrystallization annealing will not by the alpha anneal. If the alpha-anneal temper-
remove the anisotropy of the crystal structure ature is low, the precipitation of the compounds
produced by the rolling and forming processes. is fine and well dispersed.
The stock for most forming operations is pro- Figure 5(a) shows fine U3Si precipitates in a
duced by “square rolling,” or by giving the U-400 ppm Si-200 ppm iron alloy after a beta
rolled plate essentially equal reductions in the quench and 625
C (1160
F) anneal. Finer pre-
longitudinal and transverse directions. This pro- cipitation is evident in a U-200 ppm iron alloy
Fig. 1 Recrystallization temperature as a function of
cess produces a plate with relatively uniform annealed at 600
C (1110
F), as exhibited in
cold work for rolled depleted uranium of
moderate purity. Annealing time, 1½ h. Source: Ref 1 properties in the plane of the plate. Equal Fig. 5(b). After this fine precipitate dispersion
reductions taken at 45
to the standard longitu- is achieved, a second beta quench can be more
dinal and transverse directions will produce effective as a grain-refining step. Two beta
even more uniform forming stock. quenches and two alpha-annealing cycles will
Cast Uranium. The grain size of cast ura- produce the desired grain structure in stock as
niun is difficult to define because the large cast thick as 32 mm (1.25 in.) (Fig. 4).
grains all have well-organized substructures The specific details of the recommended beta
(Fig. 3). The cast micro-structure and mechani- heat treatment—such as temperature, time,
cal properties can be improved by beta heat quenching procedure, and furnace conditions—
treating (Fig. 4). In this process, the casting is are dictated by the final metallurgical condition
heated to approximately 740
C (1365
F), desired. When beta heat treating is followed by

Table 4 Typical room-temperature mechanical properties of uranium in various conditions

Yield strength(a) Tensile strength
Reduction
Fabrication history MPa ksi MPa ksi Elongation(b), % in area, %

Cast 207 30 448 65 5 10

Gamma extruded 172 25 552 80 10 12
Beta rolled 207 30 586 85 12 ...
Alpha extruded, 600
C (1080
F) 207 30 621 90 15 ...
Alpha rolled at:
300
C (570
F) 759 110 1172 170 7 14
500
C (930
F) 414 60 897 130 20 ...
600
C (1080
F) 276 40 759 110 20 ...
Annealed, sifter rolling at:
300
C (570
F) 345 50 759 110 5 ...
500
C (930
F) 276 40 690 100 15 ...
Fig. 2 Average grain size of depleted uranium as a
Beta treated after alpha rolling:
function of annealing temperature. 1 h anneals
after 50% reduction by rolling at 300
C (570
F). A and Water quenched 241 35 586 85 10 12
Slow cooled 207 30 414 60 7 ...
B are impure metal; C, D, and E are high-purity uranium
in decreasing order of submicroscopic inclusion content. (a) At 0.2% offset. (b) In 50 mm (2 in.)
Source: Ref 2

Fig. 3 Typical grain structure of cast depleted uranium Fig. 4 Microstructure of cast depleted uranium refined by beta quenching

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 670 / Heat Treating of Other Nonferrous Alloys

Fig. 5 Micrographs showing precipitates in dilute-impurity uranium alloys after beta solution treatment of 730
C (1345
F) for 30 min followed by water quenching and an aging
treatment. (a) U3Si precipitates in a U-400 ppm Si-200 ppm iron alloy after a beta quench followed by an aging treatment of 625
C (1160
F) with furnace cool. (b) Fine
precipitation in a U-200 ppm iron alloy after a beta quench followed by an aging treatment of 600
C (1110
F) for 20 h with a furnace cool

water quenching, the uranium lattice undergoes Table 5 Typical tensile properties versus heat treating methods for cast uranium
heavy strain as a result of the beta-to-alpha Tensile Yield Charpy impact
transformation. This transformation can occur Reduction
strength strength(a) J-integral energy
Elongation(b), in area, Tearing
by diffusion, massive, or martensitic mechan- Heat treating methods MPa ksi MPa ksi % % J/mm2 in.  lb/in.2 modulus J ft  lbf
isms, depending on the severity of quenching. ... ... ... ... ... ...
As-cast 420 61 205 30 6
At slower cooling rates, the beta-to-alpha trans- Vacuum heat treated, 450 65 215 31 5 ... ... ... ... ... ...
formation occurs by diffusion. A massive trans- 640
C (1185
F), 1h
formation mechanism has been shown to Vacuum heat treated, 565 82 185 27 13 ... ... ... ... ... ...
dominate at intermediate quench rates of 20 to 650
C (1200
F), 2 h,
then 630
C (1195
F),
100
C/s (35 to 180
F/s), whereas a martensitic 24 h
reaction has been observed for the most rapid Salt annealed 450 65 215 31 8 ... ... ... ... ... ...
quench rates in the dilute-impurity alloys. In Beta quenched, vacuum 785 114 295 43 22 17 0.034 192 35 14(c) 14(d)
general, to relieve the residual stresses induced annealed
0.016 90 11 7(d) 5(c)
by beta quenching and to precipitate a fine dis-
(a) At 0.2% offset. (b) In 50 mm (2 in.). (c) 54
C (129
F). (d) 21
C (70
F)
persion of secondary compounds, an annealing
temperature of 575
C (1065
F) is used. Typical
tensile properties that can be developed by vari-
ous heat treatments in cast and wrought uranium Table 6 Typical tensile properties versus heat treating methods for wrought uranium
are shown in Tables 5 and 6, respectively.
Tensile strength Yield strength(a)
Method of heat treating MPa ksi MPa ksi Elongatlon(b), % Reduction in area, %
Dilute Alloys of Depleted Uranium Vacuum heat treated 800 116 270 39 31 28
Salt annealed or short vacuum heat treated 655 95 272 39 12 12
Vacuum arc melt, vacuum heat treated 780 113 215 31 49 ...
Dilute alloys that are heat treated in Vacuum heat treated plate 835 121 273 40 40 ...
larger quantities are DU-(0.70–0.85)wt%Ti Salt annealed 885 128 215 31 20 ...
and DU-2wt%Mo. Both are used as cores in (a) At 0.2% offset. (b) In 50 mm (2 in.)
kinetic energy penetrators. The ability of these
alloys to age harden is related to the fact
that titanium and molybdenum have extended
solid solubility in the high-temperature gamma quench rate. The grain boundaries visible in treating in the gamma-phase temperature range
phase and essentially complete insolubility in the structure are those of the prior-gamma of 800 to 850
C (1470 to 1560
F), quenching
the low-temperature alpha phase. On rapid grains. The U-0.75Ti alloy is shallow harden- to room temperature, and aging in the alpha
quenching, the gamma transforms martensiti- ing, however. At the center of the bar, transfor- temperature range. Solution heat treatment is
cally to supersaturated alpha prime. A fine dis- mation to alpha phase plus U2Ti starts at prior usually done in vacuum or an argon atmosphere
persion of intermetallic compound develops grain boundaries (Fig. 6b). Similar structures for oxidation control and hydrogen outgassing.
during subsequent aging at temperatures above are found in 18 mm (0.7 in.) diam bar oil Alternatively, interrupted quenching in a mol-
300
C (570
F). quenched from the gamma phase. Aging to ten metal or salt bath held at the appropriate
Figure 6 shows the microstructure of water- peak hardness produces no detectable change temperature can be used.
quenched 36 mm (1.4 in.) diam U-0.75Ti bar. in structure. A completely gamma-phase microstructure
The outside of the bar (Fig. 6a) has transformed Solution Treating and Aging. Heat treating can be produced in a very short time, 2 to
completely to lenticular alpha prime. The fine- for improved hardness and mechanical proper- 5 min, depending on the thickness. Longer
ness of this structure increases with increasing ties in dilute DU alloys consists of solution solution heat treatment times of 4 to 8 h are

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 Heat Treating of Uranium and Uranium Alloys / 671

generally used for thicker components and for scatter) are best obtained when H2 levels are DU alloys should be similar. Because DU-Ti
hydrogen outgassing. Excessive soak times lead maintained at 0.1 ppm or less. alloys are quench-rate sensitive (shallow hard-
to unfavorable, large gamma grain sizes that Erratic ductile behavior in U-0.8Ti can be off- ening), higher quench rates are needed to
influence the final martensite lath size obtained set by controlling the effects of hydrogen by achieve uniform hardening response in large-
upon water quenching. reducing the internal hydrogen content from diameter bars or thicker plates.
An important consideration in the selection 0.36 to 0.02 ppm H2 and testing in dried air con- Effect of Quench Rate on Microstructures.
of conditions for gamma solution treatment is taining less than 10% relative humidity. A recent Figure 8 shows the effect of quench rate on
the hydrogen level required in the final product. study (Fig. 7) showed a 50% improvement in the microstructures developed during quenching.
Although hydrogen is detrimental to ductility in ductility with no loss in strength. Scanning A truly 100% martensitic microstructure can be
the U-0.75Ti alloy, acceptable ductility with electron microscopic evaluation of the fractured obtained only in very thin, rapidly quenched
occasional low values can be achieved with tensile specimens revealed a correlation of pre- samples (<3 mm or 0.12 in.), as shown in
H2 levels below nominally 1 ppm. However, mature failures originating at inclusion clusters, Fig. 8(a). Even after excessive etching (as evi-
higher and more consistent properties (less identified as titanium carbides and/or uranium denced by pitting at the grain boundaries), the
oxides. These results indicate that as the hydro- a0 martensite is not resolvable in bright-field
gen content increases, there is a greater likeli- optical micrographs but is easily detected under
hood of premature or erratic fracture at an polarized light conditions. As the quench rate is
inclusion cluster or other defect. As expected, reduced (or the quenching blank becomes more
large defects or inclusion clusters cause a signif- massive), some equilibrium a + d is formed
icant loss in ductility regardless of the hydrogen preferentially at prior-g grain boundaries and
level. Unalloyed uranium and uranium alloys are along martensite lath interfaces.
sensitive to hydrogen and, for maximum mate- Figure 8(c) represents typical acceptable
rial properties, require extensive outgassing. microstructures in a satisfactorily quenched
The literature should be consulted before select- U-0.8Ti alloy sample. The martensite laths are
ing conditions for these alloys. visible in bright field due to the interface deco-
Quenching. Table 7 gives the rates at which ration by the equilibrium a + d. Despite the
DU-0.75Ti cools when quenched in various rapid phase decomposition upon quenching,
media. The test slugs used for measuring these acceptable properties can be achieved in aged
rates were 22 mm (0.875 in.) in diameter by U-0.8Ti alloy components with up to 50% of
21 mm (0.845 in.) long. Cooling rates for other the a + d transformation products within the inte-
rior of the test specimens. On the other hand, the
U-6Nb alloy is not a quench-rate-sensitive alloy.
The a00 martensite microstructure and desirable
properties can be obtained after a gamma solution
heat treatment even at cooling rates as slow as
10
C/s (20
F/s).
Void Formation. Small-diameter bars and plates
can be plunge quenched, but larger-diameter
(a)
100 µm bars (greater than 19 mm, or 0.75 in.) develop
centerline voids if plunge quenched. These
voids pose a particularly serious problem.
Once they are formed, there is no easy way
to heal them. Void formation is related to the
stresses caused by the large volume change
associated with the gamma-to-alpha-prime
transformation and high radial thermal gradi-
ents. Centerline voids can be minimized by
end quenching—that is, by lowering the bars,
end on, at a controlled rate, into the quench
media. Bars 36 mm (1.4 in.) in diameter have
acceptable levels of centerline voids when
Fig. 7 Effect of hydrogen content and strain rate on the quenched in this way, 18 at a time, into circu-
ductility of a conventional tensile test for the lating water at 455 mm/min (18 in./min). The
U-0.8Ti alloy. RA, reduction in rate; TE, total elongation number and size of centerline voids, as
in 16.3 mm (0.64 in.) gage length
detected by ultrasonic techniques, are substan-
tially lower in bars end quenched at 255 mm/min
(10 in./min). A typical quench crack in the U-0.8Ti
Table 7 Cooling rates for DU-0.75Ti in alloy that occurred during a sluggish quenching
various quench media operation is shown in Fig. 9. Note the lack of
a0 martensite platelets along the surface where
Quench rate



the crack originated. The aging response of the
Media C/s F/s
(b) more slowly quenched bars is identical with
100 µm Flowing argon 3.8 6.8 those quenched at 455 mm/min (18 in./min).
Conventional or soluble oil 38–40 68–72 Quenching-Induced Residual Stresses and
0.05% PVA(a) 80 145
Fig. 6 Microstructure of solution-treated and
Water 98 175 Stress Leveling. Quenching high-strength ura-
quenched U-0.75Ti. Bar 36 mm (1.4 in.) in
diameter and quenched into water at 455 mm/min 10% brine 190 340 nium alloys results in extremely high residual
(18 in./min). Chrome-acetic electroetch. Original magnifi- (a) Polyvinyl alcohol
stresses that approach, and in some instances
cation: 100. (a) Edge. (b) Center exceed, the yield strength of the base

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 672 / Heat Treating of Other Nonferrous Alloys

material. The large thermal gradients during

quenching coupled with the significant differ-
ence in yield strength between the parent (g)
and product phases (either a0 or a + d), and
the phase-transformation-related volume con-
tractions, induce these large residual stresses.
The former are responsible for approximately
80 to 90% of the residual stresses, while the
latter contribute only between 10 and 20%
of the quenched-in residual stresses. These
latent residual stresses can be detrimental in
terms of delayed fracture through stress cor-
rosion or by significant distortion during
subsequent machining operations. At times,
elaborate machining procedures must be fol-
lowed to obtain a final part that will meet
drawing tolerances.
An example of the residual stresses obtained
in a U-0.8Ti alloy cylinder after immersion
water quenching is shown in Fig. 10(a). Essen-
tially, a biaxial stress state is obtained with very
high surface compressive and interior tensile
residual stresses being reached. Several
approaches have been used to reduce these
stresses prior to final machining operations.
These include thermal stress relief by aging
and stress leveling through plastic deformation.
Figure 10(b) shows that a typical aging heat
treatment (385
C, or 725
F, for 4 h + water
quench) after water quenching can reduce resid-
ual stresses by approximately one-third. On the
other hand, stress leveling by imparting 1.5%
permanent plastic axial deformation essentially
eliminates the hoop stress and dramatically
reduces the axial residual stress by two-thirds
(Fig. 10c).
Schematically, stress leveling is shown in
Fig. 11 for a compressive deformation cycle.
Upon compressive loading, the very high tensile
residual-stress point 1A follows the loading path
to 1B, whereas the large (already yielded) com-
pressive residual-stress point 2A moves to 2B.
Upon unloading, after this permanent deforma-
tion cycle, point 1B moves to 1C and 2B moves
to 2C. These new residual-stress values are sig-
nificantly reduced in comparison with the origi-
nal quenched-in residual stresses, as verified
through the experimentally measured data pre-
sented in the example (Fig. 10c).
Aging after stress leveling did not result in
any further appreciable reduction in residual
stresses. A general rule of thumb is that 2%
permanent axial deformation will provide the
optimum reduction in residual stresses in both
the axial and hoop (due to a Poisson effect)
directions. The deformation can either be ten-
sile or compressive to obtain the residual-
stress-reducing benefits. A side benefit of the
axial compressive deformation in a cylinder is
the increase in tensile yield strength in the hoop
direction and an increase in the axial compres-
sive yield strength with essentially no ductility
loss. Geometric constraints (specimen geome-
try) limit the use of the stress-leveling method
of reducing quenched-in residual stresses.
Fig. 8 Effect of quench rate on the microstructure of a U-0.8Ti alloy as seen in bright-field and polarized light optical Aging Results. Hardness and strength levels
micrographs. (a) 100% a0 martensite microstructure for a quench rate >400
C/s (>720
F/s).
(b) Microstructure developed at a cooling rate of 360
C/s (650
F/s) with <100% a0 . (c) Approximately 90% a0
achieved on aging of dilute DU alloys are illu-
martensite developed at a <100
C/s (<180
F/s) quench rate strated in Fig. 12 to 14. The hardness curves

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 Heat Treating of Uranium and Uranium Alloys / 673

for U-0.75Ti apply equally well to oil-quenched The heat treater has a wide selection of time- the prior-a0 martensite plate boundaries during
and water-quenched material (Fig. 12). The temperature options to achieve specified combi- overaging of the U-0.8Ti alloy. In contrast for
scatter band is caused by nominal differences nations of hardness and strength. For example, the U-2Mo alloy, the banded a0 martensite plate
in titanium and trace element contents of the U-0.75Ti can be hardened to 45 HRC by any boundaries do not act as preferential sites for
alloys; iron and copper, even at low levels, con- of the following treatments: 16 h at 380
C the brittle intermetallic during overaging, and
tribute to the hardening response. Silicon is (720
F); 5 h at 400
C (750
F); or 13/4 h at so higher ductility is achievable in overaged
reported to retard hardening. Aging is usually 420
C (790
F). For production runs, conditions microstructures.
done in an inert atmosphere such as argon are selected to optimize equipment utilization. A general comment on the heat treatment of
to minimize oxidation and hydrogen effects. Uranium alloys can differ significantly in uranium alloys is that the elastic moduli (tensile
A vacuum can be used but does not normally their aging response, as shown in Fig. 15. and shear) can be varied significantly (over
provide the dynamic heat flow of circulated Whereas the U-2Mo alloy develops better 100%) through heat treatment. This fact has been
argon, because aging treatments are at rela- strength/ductility combinations in the over-aged used as the basis for a quality-control method
tively low temperatures, where thermal radia- condition, the U-0.8Ti alloy must be used in the through measurement of elastic ultrasonic wave
tion (a T4-dependence) is not as effective for underaged condition because the overaged con- response to verify heat treatment. This ability to
heat transfer as conduction and convection. dition exhibits poor ductility. A semicontinuous vary modulus is opposite in behavior to conven-
film of brittle intermetallic (U2Ti) forms along tional ferrous alloys, which yield the same mod-
uli independent of heat treatment.
Mechanical Testing. External hydrogen can
lead to premature failures in U-0.8Ti. Ideally,
the test atmosphere should be one with low rela-
tive humidity, such as dried air, vacuum, or
immersed in a suitable oil. Strain rate also plays
a role in determining mechanical properties, espe-
cially ductility. Faster strain rates tend to improve
reduction-in-area values significantly (Fig. 7).
Fracture morphologies change from a mixed
mode of quasi-cleavage and micro-void coales-
cence to one of predominantly dimpled rupture.

Metastable High Alloys

Heat treatment of DU alloys with 4.0 wt% or

more molybdenum or equivalent is similar to
that for dilute alloys. The treatment starts with
a gamma-phase solution treatment of 1 h at
approximately 800
C (1470
F). This is fol-
lowed by either quenching to room temperature
followed by aging in the alpha region or
quenching directly to the aging temperature
and holding to achieve the desired properties.
Fig. 9 A poorly transformed microstructure developed by a sluggish quench can result in a quench crack for the U-0.8Ti
For higher ductilities, it may be necessary to
alloy. Acicular needles are the desired a0 martensite microstructure, while the grayish regions are the undesirable
equilibrium a + d microstructure. cold work the U-6wt%Nb alloy prior to heat

Fig. 10 Residual stresses measured by a neutron diffraction technique in a U-0.8Ti alloy cylinder. (a) After a gamma solution heat treatment and water immersion quench, a
biaxial stress state is observed with very large surface compressive and interior tensile residual stresses. (b) Aging after a gamma solution heat treatment and water
quench provides only a moderate reduction in the residual stresses from the original quenched values. (c) Stress leveling with 1.5% permanent axial compressive deformation
significantly reduces the residual stresses in a quenched U-0.8Ti alloy cylinder. Source: Ref 3

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 674 / Heat Treating of Other Nonferrous Alloys

treatment. Swaging of rods at room temperature uranium: molten baths, inert-atmosphere fur- Vacuum Treatment. Vacuum heat treating of
prior to heat treatment resulted in a slightly naces, and vacuum furnaces. The type of fur- uranium provides the best overall environment for
smaller grain size along with a 20% improve- nace chosen depends primarily on desired final obtaining maximum tensile properties and high-
ment in yield strength. Special care must be properties and material quality. quality metal surfaces. The principal advantage
taken in heat treating large sections. Cracking Uranium has been heated in molten lead for 50 of vacuum-furnace heat treating is the potential
has occurred in billets of U-6wt%Nb 200 mm h at 350
C (660
F) with no appreciable reaction. for removing hydrogen from the metal.
(8 in.) in diameter (or larger) that were water Longer periods and/or temperatures of 800 to Figure 17 shows the time required for vacuum
quenched from 800
C (1470
F). 1000
C (1470 to 1830
F), however, have caused heat treating uranium stock of different thick-
uranium to be completely penetrated. Molten nesses to achieve maximum ductility. This illus-
Processing and Equipment salts are the most common heating media used tration assumes an initial hydrogen concentration
in industry for preheating uranium prior to fabri- within the part of 2 ppm, which is typical of mate-
cation operations and for final heat treatment. rial processed through carbonate preheating
Generally, three basic furnace designs are Table 8 shows corrosion results for six heat treat- baths, and it can be used for cast material.
used for heating or heat treating of unalloyed ing mixtures of salts. The main disadvantage of A vacuum of 40 kPa (300 torr) limits oxida-
molten salt baths is the potential for hydrogen tion to an acceptable level while maintaining
contamination. Consequently, any planned use the hydrogen at its initial level. A vacuum of
of molten salt baths for heating of uranium 103 Pa (105 torr) is needed for significant
should include a design for removing the hydro- lowering of the hydrogen level.
gen from the bath, such as sparging the bath with Cleaning. Surfaces of parts to be heat treated
CO2 gas. Hydrogen, which is particularly delete- should be free of moisture, grease, and cutting
rious to uranium, drastically reduces its tensile lubricants. Heavier oxides that form on DU and
elongation, as shown in Fig. 16. its alloys can be removed by pickling for approx-
Furnace Atmospheres. No apprciable attack imately ½ h in a 1:1 mixture of nitric acid and
on uranium occurs in dry furnace atmosphere of water at 25
C (75
F). Copper, which is often
helium, argon, carbon monoxide, carbon diox- used as cladding during fabrication, can also be
ide, or hydrocarbon gases at temperatures up removed with 1:1 nitric acid. U-0.8Ti should be
to 500
C (930
F). However, relatively slight coated with a suitable oil such as MIL-C-
amounts of water vapor in any of these gases 16173D, grade 3 or stored in a dry environment
can cause extensive corrosion. Uranium reacts to mitigate the deleterious effects of hydrogen.
with water, in either liquid or vapor form, to CAUTION: Uranium-niobium and uranium-
produce UO2 and hydrogen. The UO2 spreads zirconium alloys can produce explosions during
over the entire surface area as a black powder pickling in nitric acid. The problem can be
and, depending on the amount of exposure and eliminated by adding 1 to 2 vol% of hydrofluo-
purity of the metal, can result in excessive ric acid to the pickling solution.
pitting and surface cratering. Thus, in heat Quenching. The oil-quench medium can
treating of uranium in atmospheres of commer- be contained within the vacuum chamber. Fol-
cial inert gases, furnaces should be equipped lowing solution treating, the furnace is back-
Fig. 11 Schematic of the principles of stress-leveling with gas line dryers to dry the gas thoroughly filled with argon or helium. The work is then
method of residual-stress reduction
before it is used. transferred to a position directly over the

1700
240
1600
50 Tensile strength 220
1500

1400 200

1300
180
Stress, MPa

1200

Stress, ksi
1100 160
Hardness, HRC

1000 140
40 Yield strength
Oil quenched
900
2 5 16 48
120
Water quenched 425 °C (795 °F) 800
2 5 18 42 90
2 5 16 48 2 5 16 48 700 380 °C (715 °F) 100
400 °C (750 °F) 550 °C (1020 °F)
2 5 18 42 90 2 5 18 42 90
Aging time, h 2 5 16 48 2 5 16 48 600 300 °C (570 °F) 400 °C (750 °F)
Aging temperature 380 °C (715 °F) 80
500 °C (930 °F) Unaged 2 5 18 42 90 2 5 18 42 90
335 °C (635 °F) 455 °C (850 °F)
2 5 16 48 2 5 16 48
350 °C (660 °F) 500 °C (930 °F) Aging time, h 2 5 18 42 90 2 5 18 42 90 5 42
Aging temperature 355 °C (670 °F) 500 °C (930 °F) 600 °C (1110 °F)
30

Fig. 12 Effects of aging time and temperature on hardness of U-0.75Ti

Fig. 13 Effects of aging time and temperature on tensile and yield strengths of
U-0.75Ti. Source: Ref 4

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 Heat Treating of Uranium and Uranium Alloys / 675

1700
Table 8 Corrosion of uranium in molten
240 salts at 595
C (1100
F)
1600 Tensile strength
Salt mixture Time, h Observed attack
220 44Na2CO3-30K2CO3- ½–2 No corrosion
1500
26Li2CO3
4 Surface pitting
1400 200 74K2CO3-26Li2CO3 ½–2 No corrosion
4 Pitted
1300 47Na2CO3-32K2CO3- ½–2 No corrosion
21Li2CO3
180
Stress, MPa

2 Pits beginning
1200

Stress, ksi
4 Badly pitted
160 53K2CO3-46.6Li2CO3 ½–1 No corrosion
1100 2 Surface pits
20NaOH-30K2CO3- ½–4 Surface etching
1000 50Na2CO3
Yield strength 140 47Na2CO3-47K2CO3- ½ Scaling, 0.24% weight
6Li2CO3 loss
900
2 Scaling, 1.0% weight
120 loss
800 4 Scaling, 1.3% weight
2 5 18 42 90 loss
700 355 °C (675 °F) 100
2 18 90 2 5 18 42 90
600 200 °C (390 °F) 400 °C (750 °F)
80

Elongation in 50 mm (2 in.) %
Unaged 2 5 18 42 90 2 5 18 42 90 40
250 °C (480 °F) 455 °C (850 °F)

Aging time, h 2 5 18 42 90 2 5 18 42 90 30
Aging temperature 300 °C (570 °F) 500 °C (930 °F)

20
Fig. 14 Effects of aging time and temperature on tensile and yield strengths of U-2.0Mo

10

0
0 0.2 0.4 0.6 0.8 1.0
Hydrogen content, ppm

Fig. 16 Elongation versus hydrogen content for

wrought depleted uranium

Fig. 15 Comparison between aging responses of U-2Mo and U-0.75Ti alloys

quench tank and lowered at a controlled rate treating, the quench tank is moved under the
into the quench medium. furnace. The furnace is then backfilled with
The high vapor pressure of water precludes argon or helium, the power turned off, and
incorporation of water-based quench media the bottom door removed. The load is dropped
into the furnace. Specially designed bottom- rapidly to a position 50 to 75 mm (2 to 3 in.)
loading furnaces have been used successfully above the water level and then is dropped at
with separate quench tanks. The sequence of a controlled rate until all of the workpiece is Fig. 17 Time required to achieve maximum ductility
in depleted uranium plate of various
events is as follows. At the end of solution submerged. thicknesses under a vacuum of 104 torr

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 676 / Heat Treating of Other Nonferrous Alloys

Fixtures. Neither DU nor its alloys are espe- Examples of Heat Treatment Licensing and Health and Safety
cially strong at gamma-solution-treating tem- Requirements
peratures. Low strength coupled with a high The following procedures are examples of
density places special requirements on fixturing heat treatment used to meet certain specifica-
to provide proper support and thus prevent sag- Possession of more than 6.8 kg (15 lb) of
tions of ultimate tensile strength, yield strength, depleted uranium in any form requires a license
ging. If possible, rods and irregular-shaped and elongation. Other work related to the heat from the U.S. Nuclear Regulatory Commission.
pieces should be placed with the long axis in treating of specific uranium alloys is given in Title 10, Part 40, of Federal Regulations
a vertical position and supported every Ref 5 to 8.
150 mm (6 in.); spans for horizontal pieces describes the steps necessary and the require-
Example 1: U-0.8Ti Alloy. A U-0.8Ti ments to obtain such a license. In addition, all
should be limited to 75 to 100 mm (3 to 4 in.). alloy is to be extruded and heat treated to pro- other local, state, and federal regulations are
Figure 18 shows a fixture used for solution duce components with 1240 MPa (180 ksi) ulti-
treating of bars 36 mm (1.4 in.) in diameter by effective as applicable.
mate tensile strength, 895 MPa (130 ksi) yield The greatest potential source of contamina-
380 mm (15 in.) long. This basket is made of strength at 0.85% extension, and 16% total tion in the heat treating area is uranium oxide.
Inconel 600. Tantalum shims are often used at elongation, with less than 0.3 ppm internal The area should be isolated from the remainder
points of contact between DU and the basket hydrogen:
material if the basket alloy contains a metallic of the plant, and everyone entering should be
element such as iron, which forms a eutectic at required to wear disposable protective foot-
 Billet is preheated in molten salt bath at wear. Smoking and eating should be restricted.
725
C (1335
F). Other common eutectics
found in heat treating DU include nickel at 630
C (1165
F) and extruded. The toxicity of depleted uranium if it enters
 Extruded billet is machined into blank that is the blood stream may result in poisoning simi-
740
C (1364
F), chromium at 860
C
(1580
F), and copper at 950
C (1742
F). Mol- solution heat treated at 800
C (1475
F) for lar to that caused by lead, arsenic, mercury,
8 h in vacuum and water quenched. or any other heavy metal.
ten-metal attack would result in extensive local  Blank is aged at 385
C (725
F) for 4.5 h in
wastage of the DU and welding to the fixture. A more detailed discussion about health and
Salt Baths. If a salt bath is used for solution argon and water quenched. safety requirements is provided in Properties
and Selection: Nonferrous Alloys and Special-
treating, the times should be kept as short as
Example 2: U-0.75Ti. Bars of DU-0.75Ti Purpose Materials, Volume 2 of ASM Hand-
possible, not only to minimize hydrogen pickup
but also to limit corrosive attack. Pieces alloy, 36 mm (1.4 in.) in diameter, are to be book, 1990. The important fact to remember is
exposed to molten chloride salts (BaCl2, KCl, heat treated to the following specifications: that each new operation or procedure involving
hardness, 38 to 44 HRC; minimum 0.2% yield uranium alloys should be individually evaluated
and NaCl eutectic) and molten carbonate salts
to determine the correct protective clothing and
(35% Li2CO3 and 65% K2CO3) at 730
C strength, 725 MPa (105 ksi); minimum elonga-
(1350
F) have lost 0.08 mm (0.003 in.) of tion, 12%; and maximum hydrogen content, equipment, dosimetry, and handling require-
1 ppm. The procedure is to: ments for that particular job. The prior proces-
thickness in 1 h. Such attack would be signifi-
sing history of the heat treatment samples
cantly more severe at 850
C (1560
F).
 Cut extruded bar stock to length is likewise important in this consideration,
Aging treatments can be carried out in recir-
culating inert gas furnaces, lead baths, lead-tin  Pickle in 1:1 nitric acid to remove copper because operations that change the state of the
uranium, such as casting, can make concerns
baths, or molten salt baths. Because the aging sheath
 Rinse and air dry about daughter-product beta radiation more
reactions are temperature sensitive, the tempera-
ture should be controlled to within +5
C (9
F)  Place rods vertically in a basket important than normal low-level alpha radiation
and preferably to within +2
C (4
F). Following  Solution treat 2½ h at 850
C (1560
F) in a associated with depleted uranium.
aging, the pieces should be either furnace cooled vacuum of 7  103 Pa (5  105 torr), or better
to 100
C (212
F) or water quenched. Oxidation  Quench into circulating water at 455 mm/ ACKNOWLEDGMENT
of DU is exothermic, and the heat generated can min (18 in./min)
make the reaction self-sustaining. Rods 18 mm  Air dry The information in this article is reaffirmed
(0.7 in.) in diameter have reached red heat when  Age 16 h at 350
C (660
F) in an inert gas from Heat Treating of Uranium and Uranium
they were not water quenched after being aged recirculating furnace Alloys, Heat Treating, Volume 4, ASM Hand-
at 425
C (795
F) in a lead pot. book, ASM International, 1991, p 928–938.
Example 3: U-6Nb Alloy. A U-6 Nb alloy
is to be formed into a hemisphere with the fol-
lowing mechanical properties: ultimate tensile REFERENCES
strength, 770 MPa (112 ksi) min; yield strength
at 0.2% offset, 360 to 485 MPa (52 to 70 ksi); 1. E.E. Hayes, “Recrystallization of Cold-
and total elongation, 25% min: Rolled Uranium,” U.S. Atomic Energy
Commission Report TID-2501, 1949
 Billet is preheated to 800 to 850
C (1475 to 2. E.S. Fisher, Recrystallization and Grain
1560
F) and forged. Growth in Uranium, in Reactor Technology
 Forged billet is homogenized at 1000

C and Chemical Processing, Vol 9, Proceed-


(1830 F) for 4 h in vacuum. ings of the International Conference on the
 Forged billet is preheated to 850
C Peaceful Uses of Atomic Energy, United
(1560
F) in molten salt bath and cross Nations, 1956
rolled into plate. 3. A. Salinas-Rodriguez, J.H. Root, T.M.
 Plate is preheated in argon furnace to 850
C Holden, S.R. MacEwen, and G.M. Ludtka,
(1560
F) and formed into a hemisphere. Nondestructive Measurement of Residual
 Hemisphere is solution heat treated to Stresses in U-0.8 wt.% Ti by Neutron Dif-
800
C (1475
F) for 1 to 2 h in vacuum fraction, Neutron Scattering for Materials
and water quenched. Science, Vol 166, S.M. Shapiro, S.C. Moss,
 Hemisphere is aged in argon at 200
C and J.D. Jorgensen, Ed., Materials Research
Fig. 18 Fixture for solution treating and end
quenching of 18 depleted uranium bars (400
F) for 2 h. Society, 1990

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 Heat Treating of Uranium and Uranium Alloys / 677

4. K.H. Eckelmeyer and F.J. Zanner, The Effect wt.% Titanium Alloy Cylinders,” Y-2355,  K.H. Eckelmeyer, “Diffusional Transforma-
of Aging on the Mechanical Behavior of U- Martin Marietta Energy Systems, Inc., June tions, Strengthening Mechanisms, and
0.75 wt.% Ti and U-2.0 wt.% Mo, J. Nucl. 1986 Mechanical Properties of Uranium Alloys,”
Mater., Vol 62 (No. 1), Oct 1976, p 37–49 8. G.H. Llewellyn, G.A. Aramayo, G.M. SAND82-0524, Sandia National Labora-
5. K.H. Eckelmeyer, A.D. Romig, Jr., and L.J. Ludtka, J.E. Park, and M. Siman-Tov, tories, 1982
Weirick, The Effect of Quench Rate on the “Experimental and Analytical Studies in  ”Health Physics Manual of Good Practices
Microstructure, Mechanical Properties, and Quenching Uranium-0.75% Titanium Alloy for Uranium Facilities,” Report DE88-
Corrosion Behavior of U-6 Wt.Pct.Nb, Cylinders,” Y-2397, Martin Marietta Energy 013620, Idaho National Engineering Labora-
Metall. Trans. A, Vol 15, 1984, p 1319 Systems, Inc., Feb 1989 tory, June 1988
6. K.H. Eckelmeyer and F.J. Zanner, The  A.R. Kaufman, Ed., Nuclear Reactor Fuel
Effect of Aging on the Mechanical Behavior
of U-0.75 wt.% Ti and U-2.0 wt.% Mo, Elements: Metallurgy and Fabrication,
SELECTED REFERENCES Wiley-Interscience, 1962
J. Nucl. Mater., Vol 62, 1976, p 37
7. G.H. Llewellyn, G.A. Aramayo, M. Siman-Tov,  J.J. Burke et al., Ed., Physical Metallurgy of  Metallurgical Technology of Uranium and
K.W. Childs, and G.M. Ludtka, “Computer Uranium Alloys, Brook Hill Publishing, Uranium Alloys, Vol 1–3, American Society
Simulation of Immersion of Uranium-0.75 1976 for Metals, 1982

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