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Ann. Rev. Mater. Sci. 1978. 8: 327-57 Quick links to online content
Copyright © 1978 by Annual Reviews Inc. All rights reserved
OF STEELS
R. A. Oriani
us Steel Corporation Research Laboratory, Monroeville, Pennsylvania 15146
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
INTRODUCTION
(1, 2), aluminum (3), titanium (4), zirconium (5), tantalum (6), hafnium (7),
niobium (8), vanadium (9), tungsten (10), molybdenum ( 1 1), and uranium
( 12). Despite the great technologic importance of hydrogen embrittlement
phenomena in all these systems and the undoubted scientific value of
exploring the similarities and dissimilarities among them, because of space
limitations this review considers only the embrittlement of steels by
hydrogen. Even in this narrower field, the l iterature is vast. This review
does not consider cyclic loading or the high-temperature attack of steels
by hydrogen where, for example, methane is generated. It concerns itself
with phenomena such as the reduction of the load-bearing capability
of high-strength steels, and the reduction of the ductility of low-strength
steels.
The emphasis throughout is on developing understanding, not on
cataloguing phenomena or on engineering information. We begin with a
brief presentation of the major theoretical points of view that have been
advanced. We proceed to describe the important properties and effects
of hydrogen in iron and steel that appear to be relevant to understanding
the embrittlement phenomena. We then discuss experiments on the
fracture of steels and the understanding that has been generated. We
conclude with an assessment of current understanding and of fruitful
avenues of further investigation.
atoms per unit area of interface. However, the advantage of this formula
tion is more illusory than real because of the necessity of using an
ad hoc assumption for dr/db at 15m•
Equilibrium Properties
Hydrogen dissolved in the lattice of iron exists predominantly in the
dissociated (monatomic) form and certainly occupies interstitial positions
(32); which of the possible interstices is occupied is still subject to
reasonable doubt [for a discussion see (33)]. The partial molal volume,
VR, of lattice-dissolved hydrogen is 2.0 em3/mole H in bee iron (34-36),
and probably not much different from this in fcc iron. The solubility of
330 ORIANI
alloying of iron with other metallic elements (except possibly gold) will
not change this situation appreciably. However, the prior adsorption of
nonmetallic elements may markedly change the adsorbability of
hydrogen ; reliable data on these effects are apparently not available.
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kinetics and the entry of the hydrogen thereby made available may be
complicated functions of the chemistry and morphology of the product
layer. It is known that both the ingress ( 1 8) and the exit (63) of hydrogen
from iron are seriously impeded by oxygen; it appears probable that the
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in the form of a thin sheet. The measurement may be carried out con
veniently by the double-cell electrochemical technique of Devanathan &
Stachurski (73), in which the output surface of the steel sheet is palladized
to decrease impediments to the exit of hydrogen. The hydrogen at the
input surface may be deposited potentiostatically or galvanostatically.
The input surface of the permeation sheet should be as similar as possible
in all characteristics to the surface of the specimen for hydrogen
embrittlement studies.
The sub�urface (i.e. below the first atomic plane) concentration, C1> of
lattice-dissolved hydrogen may be calculated from JooLjDLA, where L
and A are the thickness and permeation area of the sheet, respectively,
and DL is the diffusivity of hydrogen at the relevant temperature and in
the absence of any energetic sites at which hydrogen may be trapped.
The subsurface concentration C1 is proportional to the thermodynamic
activity at. the constant of proportionality depending on the arbitrarily
chosen reference state. The subsurface concentration is related to the
fugacity, 1H2, of gaseous hydrogen with which the subsurface layer would
be in equilibrium through a Sievert's law parameter. This is therefore
the effective fugacity, Ie, of the hydrogen-producing medium. An alterna
tive method of calculation is let JooL/cPA, where ¢ is the permeability
=
28.1 27.7
247 217
896 609
1860 987
3060 1315
6880 1955
1.25 x 104 25 10
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
determination will not be easily related to the local ai at the base of a pit
or a crack.
As described above, al is rdatable to the effective input fugacity of
molecular hydrogen. To know the maximum hydrostatic pressure that
can be generated by H-atom recombination in a void within a steel
exposed to a given value of fe in the absence of any relaxation processes,
one must know the pressure-fugacity relation for hydrogen (54, 74). This
is given in Table 1 for 25°C, We note that fH2 � PH,' The H2 gas pressure
within a cavity or microcrack in the metal cannot be larger than the
PH2 that corresponds to ai'
INTERNAL MOBILITY OF HYDROGEN In the absence of chemical and
structural features in a-iron with which dissolved hydrogen interacts
attractively, the diffusivity (7 1 , 75), about 5 x 1 0-9 m 2 jsec at 25°C, is so
large and the temperature dependence so small that the usual interpreta
tion of the latter as an activation energy of 8.0 kJ/mole H (7 1 ) with
which an energy barrier is surmounted becomes suspect. Flynn &
Stoneham (76) have considered alternative conceptual formulations for
the motion of light interstitials in metals.
Attractive interactions between various chemical and structural
singularities and dissolved hydrogen slow down its overall migration in
iron alloys, as Darken & Smith (77) first pointed out. Treatments of
this effect, to various degrees of approximation and generality, have been
carried out by them, by McNabb & Foster (78), Oriani (7 1 ), Ellerbrock
et al (79), Koiwa (80), Allen-Booth et al (81), and Pressouyre & Bernstein
(82). Because steels have many singularities with which hydrogen can
HYDROGEN EMBRITTLEMENT 335
interact and which can interact with each other, the analysis of a diffusion
experiment to give information on the important interacting features is
extremely difficult.
In 1951 Bastien & Azou (31) proposed that hydrogen may be trans
ported via entrainment by dislocations moving in response to applied
stresses, and that hydrogen dragged in this manner would move faster
and over longer distances than it could be diffusion motivated solely
by concentration gradients. Experiments by Frank (83) with mild steel, by
Broudeur et al (84) with 1 8-8 stainless steel, and by Louthan et al (85)
with iron, 304L stainless steel, and nickel, leave no doubt that hydrogen
entrainment by moving dislocations can indeed occur.
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
internal solid-solid interface compared with the very rapid diffusion away
through the matrix surrounding the inclusion. The dynamically generated
internal pressure does not seem important as a contributor to the
phenomena of hydrogen embrittlement.
Yu & Li (9 1 ) developed the idea that a stress-induced, large con
centration of dissolved hydrogeh becomes supersaturated when the stress
field is suddenly relaxed by the formation of a separation at an inclusion
matrix interface. The supersaturated, dissolved hydrogen enters the micro
void formed and exerts a large pressure, causing the microvoid to grow.
The diffusion and recombination to form molecular hydrogen must
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
of prior hydrogen charging. Cornet (94) also found that an iron showed
a residual effect of hydrogen (strained after removal of the hydrogen) only
when the permeation transient determined on that iron exhibited
anomalies.
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or configuration. A micro void may be lenticular, crack-like, etc, depending on the manner
of its origin.
338 ORlAN I
say, increasing input fugacity. Kusch ( 1 1 6) also found larger flow stresses
when iron single crystals ( 1 0 to 20 ppm C, N < 5 ppm, 0 < 5 ppm,
Si ;:;;; 100 ppm) were strained under high-fugacity hydrogen. On the other
hand, Lee et al ( 1 1 7) observed that hydrogen caused a lowering of the
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stress and the rate of work hardening, do/de, of zone-refined iron. How
ever, in the domain of larger plastic extensions, hydrogen increases both
the flow stress and do/de. Working with polycrystals, Gourmelon ( 1 2 1 ,
1 22) decomposed the flow stress into the thermal and athermal com
ponents by a procedure that implies identity between the effective stress
(that which is effective in causing motion of dislocations) and the thermal
component. The result of this analysis is that for low e the thermal
component is raised by hydrogen but the athermalls strongly decreased,
whereas at larger values of e, where multiple slip becomes important,
both components are raised by hydrogen. These studies were comple
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
Hydrogen-Assisted Fracture
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
hydrogen to that without hydrogen. The plot has two branches. One
branch, with r ranging from unity to 0.2, represents data for fcc iron
and nickel alloys with hydrogen at moderate values of supersaturation.
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The other branch, from unity to 1.6, has only two data points, one from
(127) with very-high-fugacity hydrogen, and one for Ni-2Th0 2 from un
published work by Thompson. The branch for r < 1 can be un
ambiguously ascribed to a nucleation enhancement of microvoids by
hydrogen, presumably by hydrogen's decreasing the force needed to
rupture bonds across the inclusion-matrix interface. The branch for
r > 1 must be ascribed to an enhancement of void growth by hydrogen,
probably by the internal pressurization effect referred to by Garber et al
( 134). It would clearly be important, because unexpected, to find cases
where r > 1 in the absence of any possibility of an internal pressurization
effect.
Small amounts of impurities can change the path of hydrogen-assisted
cracking. Cornet (94) found that carbon added to very pure zone-refined
iron under externally applied stress and with cathodically charged
hydrogen changes the crack path from intergranular to transgranular.
The same behavior has been found for nitrogen ( 122). Bernstein (97)
found a similar effect of carbon upon the crack path of purified irons
subjected to high-fugacity charging without an externally applied
mechanical load. He also found that the crack path could be varied
reversibly from inter- to transgranular by suitable variation of the thermal
history or of the concentration of interstitial solutes, and that for any
one specimen the crack path under hydrogen charging was the same as
that observed after low-temperature tensile straining in the absence of
hydrogen. Addition of silicon to an Fe-C alloy inverts the intergranular
transgranular crack-path transition caused by carbon (127). In a high
strength Cr-Mo alloy (1 36), increasing the amount of dissolved nitrogen
changes the predominant mode of failure under tensile loading with
cathodically charged hydrogen from trans- to intergranular.
It is often possible by suitable thermal treatments to produce cracking
HYDROGEN EMBRITTLEMENT 345
paths that are the same both for low-temperature straining or impact
testing without hydrogen and for hydrogen-assisted cracking at room
temperature. Bernstein et al (127) used the same heat treatments on Sb
doped Fe-C alloy as those used on it by Rellick & McMahon ( 1 37)
and found that high-fugacity hydrogen, without externally applied load,
produced cracks along the same loci, different for each heat treatment,
as those produced by low-temperature tension ( 137). Similarly, Yoshino
& McMahon ( 1 38) found that the heat treatment that causes HY 1 30
steel to embrittle and fail intergranularly by impact in the absence of
hydrogen causes that steel to undergo a change from trans- to inter
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
steel. Viswanathan & Hudak (128) also applied Auger electron spectro
scopy to impact-fracture surfaces of 4340-type steel that had been temper
embrittled ; they inferred that the greater susceptibility to gaseous H 2 S
cracking of such steel was due to segregation of P and Ni.
Fractographic work has demonstrated that in many cases, especially
in lower-strength steels, hydrogen can have marked effects on macro
scopic ductility without producing a qualitative change in the ductile
appearance of the fracture surface. The quantitative changes therein must
be investigated further. Impurities acting singly or synergistically can
change the crack path in iron and iron alloys exposed to high-fugacity
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
cracked specimens in contact with aqueous systems, and it has not been
met with precharged specimens.
The most scientifically useful experiments are those done with gaseous
hydrogen, especially where great care has been taken with the purity of
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the gas. The work of Williams & Nelson (61) with fully hardened 4 1 30-
steel and Hz gas in the region of about 1 atm pressure demonstrated
for the first time that the logarithm of crack velocity, v, vs reciprocal
temperature, at constant K and Hz gas pressure, p, is an inverted U
curve, and that the function v(p) has different forms in the various
temperature ranges of the U-shaped curve. This complex behavior has
been corroborated by others ( 1 32, 1 46-148), and was explained (61) in
terms of chemisorption kinetics. Although the specific model used by
these authors has been shown (149, 1 50) not to agree with the experimental
results, the idea that the rate-controlling step is at the gas-metal interface
is in all probability correct (24), and is greatly strengthened by the later
work of Nelson et al (62). These investigators found that with partially
dissociated hydrogen gas the log v(1/T) curve is a straight line continuing
to rise in the temperature domain in which with molecular hydrogen
there is a downturn in the log v(IIT) curve (61). Clearly, the dissociation
of the H2 molecule must be at least one of the kinetically controlling
steps in the higher-temperature branch of the U-shaped curve. The kinetic
details of the gas-to-subsurface process have yet to be experimentally
elucidated. The alloy composition will probably be found to affect the
various kinetic steps.
Simmons et al (142) found that the activation energy for crack growth
in 4340-steel, in which the environment in contact with the crack surfaces
is pure water, is the same as that for the reaction of water vapor with
the steel to form oxide, as followed by Auger electron spectroscopy. This
suggests that the oxidation reaction that produces the hydrogen respon
sible for the embrittlement is the rate-limiting process in this case.
At constant environmental conditions the log v(K) curve is generally
found to be composed of three stages ( 1 39, 1 46, 1 5 1-1 54). At low K there
348 ORIANI
measurements, and was found to agree roughly with that which may be
deduced from the theory. The temperature dependence is in qualitative
agreement with the finding of Gangloff & Wei (1 32) that a small increase
of temperature causes a crack in 1 8-Ni maraging steel to become static
and a small decrease in temperature causes it to propagate.
That there should be some unique relationship between the macro
scopically measurable stress intensity parameter K and the maximum
stress in the region of the crack tip for a given steel is physically
reasonable for a slowly moving crack, as long as K is either constant
or is monotonically increased. The relationship will be different, however,
if the applied K (or load) is decreased, or if the crack has been put in
Annu. Rev. Mater. Sci. 1978.8:327-357. Downloaded from www.annualreviews.org
predominantly occurs deep within the plastic enclave and that the
necessary non-Hookean stresses are generated via dislocation interactions.
How these large, highly localized stresses may be related to macro
scopically measured parameters such as K is an unsolved problem in
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mechanical metallurgy.
Another weakness of the current expression of the decohesion theory
(22) is its inability to explicitly consider the role of interfaces in the
steel that are structurally weaker than the matrix, where hydrogen
aggravates an already vulnerable situation. The role of interfaces was
appreciated in the early formulation of the model (24), and their im
portance has been seen in some of the experimental work described in
earlier sections of this review. However, an explicit, operationally useful
formulation of the role of the interfaces has yet to be incorporated into
the decohesion model.
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3 56 ORlAN I
CONTENTS
PREFATORY CHAPTER
RESOURCES AND THE QUALITY OF LIFE IN 2000, Harvey Brooks
SPECIAL MATERIALS
NEW HIGH-PERFORMANCE PERMANENT MAGNETS BASED ON RARE EARTH-
TRANSITION METAL COMPOUNDS, A. Menth, H. Nagel, and R. S. Perkins 21
SEMICONDUCTORS FOR PHOTOELECTROLYSIS, L. A. Harris and R. H. Wilson 99
MATERIALS FOR INTEGRATED OPTIcs: GAAs, Esther M. Conwell and Robert D.
Burnham 135
DATA SOURCES
DATA SOURCES FOR MATERIALS SCIENTISTS AND ENGINEERS, J. H. Westbrook
and J. D. Desai 359
INDEXES
Author Index 497
Subj ect Index 510
Cumulative Index of Contributing Authors, Volumes 4-8 521
Cumulative Index of Chapter Titles, Volumes 4-8 522