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A Review Paper on Aging Effects in tures.

A significant amount of data has been generated for these


applications since its development in the early 1970s. To prepare
Alloy 617 for Gen IV Nuclear the alloy for applications in Gen IV nuclear reactors, existing data
and literature of the alloy are reviewed in this paper for under-
Reactor Applications standing the aging effects and providing guidelines for further
investigations.
Weiju Ren
Materials Science and Technology Division, 2 The Material
Oak Ridge National Laboratory, The chemical composition of Alloy 617 is given in Table 1. The
MS-6155, Building 4500-S, high Ni and Cr contents provide the alloy with a high resistance to
Oak Ridge, TN 37831 a variety of reducing and oxidizing environments. Al, in conjunc-
tion with Cr, offers oxidation resistance at high temperatures. In
e-mail: renw@ornl.gov
addition, Al also forms an intermetallic compound ␥⬘ over a range
Robert Swimdeman of temperatures, which results in precipitation strengthening on
top of the solid solution strengthening imparted by Co and Mo.
Cromtech, Strengthening is also derived from M 23C6, M 6C, Ti共C, N兲, and
125 Amanda Drive, other precipitates.
Oak Ridge, TN 37831 Product forms of Alloy 617 employed in various research and
e-mail: rswindeman@comcast.net development activities reviewed in this paper include the bar, cold
drawn tube, cold rolled sheet, extruded tube, forging, flat, plate,
sheet, and wire. Among these products, bar, plate, and wire were
reported for aging and/or environmental effect studies. All these
To understand the response of Alloy 617 to long-time exposure forms were investigated for creep properties. In many cases, the
conditions and to determine the supplementary data needs for post-test evaluations of these research activities provide supple-
structural components in Gen IV nuclear reactors, literature of mental data on aging as influenced by the specific testing or ser-
aging and aging effects in the alloy was reviewed. Most of the vice conditions. Many reports also provided chemistry informa-
reviewed data were produced in connection with the international tion for the products investigated.
research effort supporting high temperature gas-cooled reactor
projects in the 1970s and 1980s. Topics considered included mi-
crostructural changes, hardness, tensile properties, toughness, 3 Research Activities and Publications
creep-rupture, fatigue, and crack growth. It became clear that, for Since the introduction of Alloy 617 in the early 1970s, research
the long-time very high-temperature conditions of the Gen IV re- programs were actively conducted on the material in several coun-
actors, a significant effort would be needed to fully understand tries, resulting in a significant amount of papers and reports. Some
and characterize property changes. Several topics for further re- major publications are briefly reviewed in this section in chrono-
search were recommended. 关DOI: 10.1115/1.2967885兴 logical order. Findings on particular topics in these publications
are discussed in Secs. 4–9.
3.1 Major Research Activities in the 1970s. In 1972, Alloy
1 Introduction 617 was introduced by Hosier and Tillack 关1兴 as a solid solution
Alloy 617 is identified as one of the candidate materials in Gen alloy with good strength for a very high-temperature service. It
IV nuclear reactor systems for components serving in the tempera- was then followed by Mankins et al. 关2兴 in 1974 with a paper on
ture range of 760– 950° C.1 The leading Gen IV reactor concept, aging effects in the temperature range of 649– 1093° C. The ma-
very high temperature reactor 共VHTR兲, is a gas-cooled reactor terial studied was a 19 mm diameter hot-rolled bar, solution
with an operational goal of producing helium at temperatures up treated at 1177° C. Samples included tensile bars aged for 50 h
to 950° C, pressures up to 7 MPa, and a design life up to 60 years. and 1000 h and post-test creep specimens ruptured from 215 h at
Several other Gen IV nuclear reactor concepts supported by the 1093° C to beyond 10,000 h at 760° C. Phases extracted from the
US Department of Energy also require high service temperatures samples were analyzed by X-ray diffraction to investigate precipi-
and long design lives. During long-term service at high tempera- tates formed during the aging process. Computer modeling using
tures, metallic materials inevitably undergo processes that involve PHACOMP was also conducted to estimate the second phases.
microstructural evolution and changes in mechanical properties. Room temperature tensile, hardness, and Charpy V-notch 共CVN兲
Such evolution and changes usually result in degradation of prop- impact tests were performed on the aged specimens to study the
erties or function with time and are normally referred to as aging. aging effects on yield strength, ultimate tensile strength, ductility,
Apparently, to select construction materials and develop design and toughness.
guidelines for the Gen IV reactors, a mechanistic understanding of By the mid-1970s, Alloy 617 became a strong candidate for
the aging effects in the candidate materials that would arise during structural components in high-temperature gas-cooled reactor de-
long-term and high-temperature exposure becomes very impor- signs. Kimball et al. 关3兴 undertook an activity to extend the aging
tant. data of Mankins et al. to a longer time. They examined a 12.7 mm
Alloy 617, also designated as Inconel 617, UNS N06617, or W. hot-rolled plate solution annealed at 1177° C and aged at tempera-
Nr. 2.4663a, was initially developed for high-temperature applica- tures from 593° C to 816° C for 168–8000 h. Post-aging evalua-
tions above 800° C. It is often considered for use in aircraft and tions included hardness, CVN impact testing, and metallographic
land-based gas turbines, chemical manufacturing components, studies. The metallography was focused on the characteristics of
metallurgical processing facilities, and power generation struc- the M 23C6 carbide formation of the continuous film of carbides at
the grain boundaries and the tendency toward a carbide denuded
zone in the matrix near the grain boundaries.
1
Reduced from the initial 1000° C consideration based on analysis results that In the 1975–1976 time frame, a research on Alloy 617 tested in
950° C can satisfy the application requirements. air and helium with various contaminants was reported by Hosoi
Contributed by the Pressure Vessel and Piping Division of ASME for publication
in the JOURNAL OF PRESSURE VESSEL TECHNOLOGY. Manuscript received October 5,
and Abe 关4兴, Kitagawa et al. 关5兴, and von der Gracht et al. 关6兴.
2006; final manuscript received April 25, 2007; published online December 30, 2008. However, their focus was mainly on the high-temperature me-
Review conducted by Noel O’Dowd. chanical behavior and helium effects rather than aging effects.

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Table 1 Chemical composition „wt %… of Alloy 617 „source: pickup increasing with time and temperature. Later, McCoy re-
Special Metals Bulletin SMC-029… ported on the aging response of modified 617 alloys 关16兴. In one
series of three modified alloys, Cr was reduced from near 22% to
Ni Cr Co Mo Fe Mn Al 16% and 12%. The variation of retained CVN energies with de-
Min 44.5 20.0 10.0 8.0 - - 0.8 creasing Cr content after aging for 10,000 h at 704° C and 871° C
Max - 24.0 15.0 10.0 3.0 1.0 1.5 was determined. Aged samples were retained in the archives at
C Cu Si S Ti B ORNL and are available for further evaluation.
Min 0.05 - - - - - In 1986, Garud 关17兴 developed a physically based model for
Max 0.15 0.5 1.0 0.015 0.6 0.006 correlating the changes in the strength and toughness of materials
exposed to HTGR environments. He considered three alloys of
interest to HTGR including Alloy 617. The emphasis was on the
nucleation, growth, and coarsening of carbide precipitates and
their influence on the deformation and microcracking processes.
A significant study of aging and effects on creep behavior at The model expressed the fracture strain in terms of microstructure
1000° C was published by Kihara et al. in 1980 关7兴. Three heats of through one term that incorporated the particle shape and a second
bar products were included. The study provided detailed informa- term that incorporated the fraction of the grain boundary covered
tion on the type, geometry, distribution, and evolution of aging by precipitates. The model was adjusted such that a “minimum” in
precipitates and their relationship with the applied stress and the toughness could be predicted as a function of aging time at a
internal oxidation. constant temperature.
3.2 Major Research Activities in the 1980s. The interna- In the late 1980s and early 1990s, research emphasis was
tional research effort on materials for gas-cooled reactors was placed on the formulation of models to represent deformation and
vigorous in the early 1980s, and in 1984, an entire issue of corrosion behavior of Alloy 617. Efforts to develop “code con-
Nuclear Technology was devoted to reviewing the progress 关8兴. struction rules” were undertaken in Germany and in the US. The
In this issue was a paper by Kirchhofer et al. 关9兴 that provided German structural design rule KTA 3221 was written but no ex-
a time-temperature precipitation 共TTP or TTT for time- plicit consideration of aging effects was included 关18,19兴. Like-
temperature transformation兲 diagram for Alloy 617. Two heats of wise, rules for the design of Alloy 617 nuclear components at a
very high temperature were drafted for the ASME Boiler and
the bar material solution treated at 1200° C followed by a water
Pressure Vessel Code but rules to handle aging effects were not
quench were examined. Aging temperatures ranged from 500° C
included 关20兴.
to 1000° C for times from 0.5 h to 1000 h to produce over 70 aged
conditions. Additional samples aged for longer times were ob- 3.3 Major Research Activities in the 1990s to Present. Sev-
tained from a companion project and produced times to 10,000– eral papers were published on experiences with Alloy 617 in tur-
30,000 h at 900° C. Precipitate characterization methods included bine applications in the 1990s 关21–24兴. The temperatures of con-
optical metallography 共OM兲, scanning electron microscopy cern were in the range of 760– 982° C and loadings included the
共SEM兲, transmission electron microscopy 共TEM兲, energy disper- creep, low-cycle fatigue, and thermal fatigue. Microstructural
sive X-ray analysis 共EDA兲, and X-ray diffraction of extracted resi- studies and aging effects were secondary to the main thrust of the
dues. Vickers diamond hardness values 共HVs兲 were also reported research, although both were briefly addressed in some of these
for aging times of 300–1000 h. papers.
In a companion research project published in this issue of Increased interest in ultrasupercritical 共USC兲 steam boiler tech-
Nuclear Technology, Bruch et al. 关10兴 aged a tubing product at nology in Europe and in the US in the 1990s produced research
temperatures from 700° C to 1000° C for times up to 30,000 h. activities on high-nickel alloys for use in boiler tubing, headers,
Their aged samples were included in the study of Kirchhofer et and piping. Alloy 617 became a leading candidate for the manu-
al., but they provided an extension of the CVN energy data. facture of boiler components that operate at 750° C 关25–27兴. Al-
Schneider et al. 关11兴 included aging effects in their examination though the temperatures of interest for USC steam boiler applica-
of the creep behavior of Alloy 617 and published in this issue of tions were lower than those of interest for the VHTR, the research
Nuclear Technology. They performed testing at 850° C and 950° C supporting the USC steam boiler development in Europe covered
for times of up to 10,000 h. Samples aged 175 h, 500 h, 3100 h, a range of temperatures to 800° C with aging treatments to
and 8700 h were tested at 950° C and 44 MPa. 1000° C. In a European project, Allen et al. 关28兴 examined the
Ennis et al. 关12兴 also published in this issue of Nuclear Tech- virgin and service-aged Alloy 617 and its weldment from a gas-
nology their observation of some aging effects in Alloy 617 dur- turbine combustion system with approximately 25,000 equivalent
ing the course of the study of helium and carburization effects on operating hours. The microstructure of the aged base metal, the
the creep behavior, tensile properties, and toughness. Their aging HV of the aged base, the weld, the outside and inside wall metals,
treatments were performed for 2000 h at 850° C. etc., were determined.
In the US, research on Alloy 617 was also vigorously con- In the US, the USC steam boiler project, a restricted chemistry
ducted for gas-cooled reactors at the Oak Ridge National Labora- version of Alloy 617 developed in Europe for USC steam boiler
tory 共ORNL兲 and other government contractor facilities. In 1982, applications, designated CCA617, was chosen for evaluation
Strizak et al. 关13兴 reported aging effects on the low-cycle fatigue 关28,29兴. Microstructural studies were conducted by Wu and Va-
at the aging temperatures of 538° C, 704° C, and 871° C for sudevan 关30兴 to examine the aging response of CCA617 relative
10,000 h and 20,000 h. McCoy and King 关14,15兴 examined aging to the standard Alloy 617 retrieved from the HTGR project at
effects in Alloy 617 and its filler metal after exposure to air, argon, ORNL. Aging conditions for the precipitate study ranged from
and a “HTGR-He” 共HTGR denotes high-temperature gas-cooled 28,300 h at 538° C to 51,850 h at 871° C. Hardness was also
reactor兲 environment. Two heats of plate product and one heat for measured for various aging conditions. The produced data were
filler wire were used, although the aging work on the wrought used by Shingledecker et al. 关31兴 to construct hardness versus
alloy was concentrated on one heat. Welds were prepared by the time curves for a broad range of temperatures and times. Informa-
gas tungsten arc process. Times for the aging in air or argon were tion on the changes in properties with aging was also provided in
2500 h, 10,000 h, 20,000 h, and 53,000 h while times for the the Inco Alloys International alloys brochure 关32兴.
aging in helium were 10,000 h, 20,000 h, and 53,000 h. Aging With the prospects for the re-emergence of VHTR technology
temperatures were in the range of 593–871° C. Samples aged at in the early 2000s, the Nuclear Regulatory Commission undertook
704° C and higher in a flowing helium environment reviews of the status of gas-cooled reactor materials and design
共15– 100 cm3 / min兲 experienced carburization with the carbon technology. Natesan et al. 关33兴 reviewed material behavior in

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4 Aging Effects on Microstructure
Alloy 617 is nominally a solid solution wrought alloy. The
ASME specification for plate products 共SB-168兲 requires solution
annealing at a minimum of 1150° C followed by water quenching
or rapid cooling by other means. Typically, a grain size of ASTM
No. 6 共45 ␮m兲 or coarser is preferred, but it has been shown that
the creep strength increases with increasing grain size so micro-
structures at 100 ␮m or 200 ␮m grain size are often produced. A
tradeoff exists, however, when fatigue is an issue since finer grain
sizes are preferred for fatigue resistance. A typical material deliv-
ered by the mill will contain some precipitates on grain bound-
aries and “clusters” of precipitates strung parallel to the rolling
direction, as shown in Fig. 1.
Fig. 1 Typical microstructure for a mill-annealed Alloy 617
THERMOCALC® was used to calculate the equilibrium phases
„Heat XX01A3US… †14‡
from 600° C to 1400° C in an Alloy 617 composition, as shown in
Fig. 2 关35兴. The M共C , N兲 forms from the melt and persists through
the entire temperature range of interest. The M 6C carbide is stable
at the solution treating temperature and is the globular precipitate
HTGR environments and provided recommendations for needed that occurs on grain boundaries and clusters. Figure 2 shows that
research and data production for a number of candidate alloys as much as 1 wt % of M 6C could be present at an annealing
including Alloy 617. Shah et al. reviewed the design technology temperature of 1177° C. It also indicates that as the temperature
including the applicable codes and procedures needed for the con- decreases, the M 23C6 starts to form below 1000° C at the expense
struction of HTGR components 关34兴. Codes and draft codes de- of the M 6C. Approximately 1 wt % could be present after a long
veloped in the US, France, and Britain were included. Observa- time at 800° C and below. The ␥⬘ 共Ni3Al兲 starts to form at around
tions were that many of the materials needed for the HTGR were 800° C and its equilibrium content increases with decreasing tem-
not included in the construction codes, the maximum temperatures perature down to 600° C where as much as 8 wt % could be
permitted in the codes were too low for the materials covered by present under equilibrium conditions.
the code, and the environmental effects were not considered in the The predictions of THERMOCALC differed significantly from
codes. A number of code actions, materials data needs, and design those of the PHACOMP analysis performed by Mankins et al. 关2兴
methodology needs were identified. Included in the needs was who estimated about 0.6% ␥⬘ in the temperature range of
research on the influences of aging on deformation and toughness. 649– 760° C. However, it was clear from the review that the ki-
In Secs. 4–9, aging effects on the microstructure, hardness, ten- netics of the precipitation and coarsening processes were impor-
sile properties, toughness, creep and stress rupture, and fatigue tant in determining the effects of aging on properties. To bring the
and crack growth will be discussed based mainly on the findings many references into a better framework for comparison, the mi-
from the research activities reviewed above. crostructural evolution will be presented on the basis of specific

Fig. 2 Content of precipitates in Alloy 617 calculated by THERMOCALC for 1.24% Al „high
aluminum… †35‡

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Fig. 3 Time-temperature-precipitation data for M23C6 carbide in Alloy 617 †2,9,30‡

precipitates, starting with those that were thought to have the solution treatment, and the carbide forms on reheating at nearly all
greatest impact on the properties. These are M 23C6, M 6C, and ␥⬘. temperatures in the creep range. This behavior differs from the
Other precipitates may be present but not abundant therefore will predictions of THERMOCALC shown in Fig. 2, but the TTP diagram
only be briefly mentioned. does not indicate the quantity, sites, or the elemental content of
M 23C6. The M 23C6 is thought to be the most abundant. Figure 3 the precipitate. The THERMOCALC analysis shows that Cr is the
summarizes the data reported by several investigators 关2,9,30兴. major metallic element in the carbide.
The legends map out the aging times and temperatures at which M 6C. The M 6C is the second most frequently observed carbide
M 23C6 was observed and/or not observed by investigators, and and occurs at higher temperatures. The TTP diagram is shown in
thus delineate the precipitation time and the temperature condi- Fig. 4. It is indicated that Mankins et al. 共Obs. 2 in the figure兲 did
tions. Rapid cooling was necessary to avoid the carbide after the not observe M 6C 关2兴. However, some details of its distribution

Fig. 4 Time-temperature-precipitation data for M6C carbide in Alloy 617 †2,9,30‡

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Fig. 5 Time-temperature-precipitation data for Ni3Al carbide in Alloy 617 †2,9,30‡

and conversion to M 23C6 are provided by Kihara et al. 关7兴 共Obs. TTP plot is provided in Fig. 5. No boundaries have been drawn to
4兲 in their study of the creep behavior at 1000° C. The M 6C car- indicate its appearance or disappearance. Kirchhofer et al. 关9兴
bide does not occur after long-time aging at temperatures below 共Obs. 1兲 found it to be present over a broad range of temperatures
900° C. Again, this behavior is inconsistent with the predictions of and times. Mankins et al. 关2兴 共Obs. 2兲 observed its “rare” presence
the THERMOCALC analysis shown in Fig. 2, although the analysis at 760° C. Wu and Vasudevan 关30兴 共Obs. 3兲 found “large
does show a decreasing presence with decreasing temperature. amounts” at temperatures below 704° C. The THERMOCALC analy-
Ni3Al. The Ni3Al intermetallic is the third most common fea- sis indicated that the temperature limit and quantity of Ni3Al are
ture of the aged microstructure. The precipitate is generally too sensitive to the composition 关35兴.
fine to be observed in optical microscopy, so the number of pa- Other phases that have been identified include the CrMo共C,N兲
pers, which provide details of its presence in Alloy 617, are few. A and TiN observed as rare by Mankins et al., the M 12C observed by

Fig. 6 Alloy 617 hardness versus log time from several investigations

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Fig. 7 Hardness versus temperature for the 1000 h aging

Kirchhofer et al. at very high temperatures, a possible Laves phase been converted to HV by means of the conversion table in ASTM
observed by Kirchhofer at long times and low temperatures, and a E 140 for nickel and high-nickel alloys. In the range of
Ni2共MoCr兲 observed by Wu and Vasudevan at long times and low 650– 800° C, significant hardening occurred. This response was
temperatures. It is not known whether any of these phases influ- probably a result of ␥⬘ precipitation but the kinetics appeared to
ence the mechanical behavior considered in the assessment of vary from heat to heat. Figure 6 plots the HV hardness against the
aging effects. log time obtained from several investigations at 700° C and
704° C. The virgin hardness values were typically in the range of
5 Aging Effects on Hardness HV 160–180. As shown in the figure, significant increases in hard-
Several hardness scales have been used by different researchers. ness developed within 100 h. Values climbed to above HV 240,
To provide comparisons in this review, all hardness values have but the heats appeared to harden at different rates. The TTP plot in

Fig. 8 Hardness versus temperature for long-time aging

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Fig. 9 Aging effect at several times and temperatures on the room temperature yield
and ultimate strengths of a single heat

Fig. 5 provided no help in estimating the time for ␥⬘ to appear h data shown in Fig. 7 indicate a peak for the heat UW material at
since not all investigators observed the intermetallic formation. 600° C 关9兴 and a peak for the material at 700° C 关3兴. In both cases
Furthermore, a “modest” increase in hardness such as that ob- the hardness falls to levels that are typical of annealed materials
served for the heat UW material 关9兴 was expected as a result of the when aging temperatures exceed 800° C. The hardness after long-
M 23C6 precipitation. time aging indicated a peak for the material near 600° C 关9兴 and
The hardness as a function of temperature is plotted in Figs. 7
the material near 700° C 关3兴. Again, the hardness fell for aging
and 8 for 1000 h and long-time exposures, respectively. The 1000

Fig. 10 Effect of aging at several times and temperatures on the room temperature
tensile elongation of a single heat

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Fig. 11 Aging effect for 1000 h at several temperatures on the room temperature yield
and tensile strengths of two heats

above 800° C and approached the virgin hardness at 900° C. It changes in the short-time properties due to long-time service.
would be of value to retrieve the archive material from the source Similar to the observations of the microstructure and hardness
关9兴 and pursue metallurgical studies to shorter times to examine behavior, the effect of aging on tensile properties is variable from
the kinetics in more detail. one heat to another and both the kinetics and magnitude of the
changes reflect this variability.
6 Aging Effects on Tensile Properties Figure 9 shows the variation in the yield and ultimate strengths
Tensile data for aged material are important in the development in a single heat aged at several temperatures for times up to
of factors that apply in the ASME Subsection NH to account for 12,000 h 关32兴. The strength increased with aging time but was

Fig. 12 Effect of aging at several temperatures at long times on the room temperature
yield and tensile strengths of two heats of Alloy 617

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Fig. 13 Effect of aging at several temperatures to long times on the room temperature
elongation of two heats of Alloy 617

sluggish at 593° C and began around 10,000 h. Hardening was 25%. The aging effect for 1000 h at several temperatures on the
more rapid at 649° C and reached a maximum before 10,000 h. At room temperature yield and tensile strengths of two heats of Alloy
704° C and 760° C, hardening was rapid but the peak strengths 617 is shown in Fig. 11. The peak in strength occurred for the
were less than for aging at 649° C. The change in elongation with material aged in the temperature range of 650– 700° C. Data for
aging time for the same heat is shown in Fig. 10. For aging at longer aging times are plotted in Fig. 12. Again, the peak in
593° C, the elongation was changed very little until the aging time strength occurred at around 650° C. A significant development,
approached 10,000 h. For aging at 649° C, the decrease occurred however, is the fact that the material investigated by McCoy and
after 100 h. A rapid loss in ductility occurred with aging at 704° C King 关14兴 exhibited a loss in ultimate strength when aged at
and 760° C. The residual elongation at all temperatures exceeded 871° C. The room temperature tensile elongation, plotted in Fig.

Fig. 14 Effect of aging at 871° C on the yield and tensile strengths and the elongation of
Alloy 617 at 871° C †14‡

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Fig. 15 Room temperature Charpy V-notch energy versus the aging time to beyond
10,000 h at four temperatures

13 as a function of aging temperature, exhibited decreasing values more research is needed to establish the lower limit for the
when aged for long times but it is not clear that the value of 20% strength and ductility at temperatures of 850° C and above.
represents a minimum. McCoy and King also performed some
tensile testing at the aging temperature. Typical data for the series
at 871° C are plotted in Fig. 14. Relative to the virgin material, 7 Aging Effects on Toughness
there was a decrease in strength, except for one unusually high The CVN impact test was used most often as a measure of
ultimate strength value for a sample aged 20,000 h. It is clear that toughness. Several sources reported the room temperature ener-

Fig. 16 Room temperature Charpy V-notch energy versus the aging temperature for
1000 h of aging

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associated with intergranular fractures, as shown in Fig. 17 关14兴.
The fracture of the same heat in virgin condition exhibited mostly
transgranular ductile shear characteristics with some intergranular
fracture segments. It is clear that more aging studies are needed at
temperatures above 800° C.

8 Aging Effects on Creep and Stress-Rupture


The aging effects observed in regard to short-time properties
such as hardness, tensile, and impact properties indicated signifi-
cant changes in microstructure during the first 10–100 h when the
exposure temperatures exceeded 650° C. Creep testing, however,
generally consumes times beyond 100 h, so it might be expected
that aging effects would “wash out” in long-time creep testing
above 650° C. Only the early stages of primary creep would be
Fig. 17 Typical fracture surface of the CVN specimen frac- affected by the simultaneous processes of creep and precipitation
tured at room temperature after long-time aging in the tempera- associated with aging. Kihara et al. 关7兴 and Schneider et al. 关11兴
ture range of 704– 871° C †14‡ studied the influence of aging on the primary creep curve. Both
noticed that the primary creep behavior of the annealed material
was somewhat complicated in the temperature range of
gies after aging. The virgin CVN energy values varied substan- 850– 1000° C. A very small period of rapidly decreasing creep
tially from heat to heat and ranged from 175 J to 325 J for five rate was followed by a period of increasing rate and then a gradual
heats in this review. Some selected data for two heats are plotted approach to a constant rate, which eventually gave way to the
in Fig. 15. These data show the CVN energies as a function of tertiary creep stage. A creep curve produced recently at 950° C
aging time to beyond 10,000 h for four temperatures. The CVN and 30 MPa shows this behavior in Fig. 18. Here, the very early
energy values dropped slowly for the 593° C exposure but more primary creep stage is missing, but the increasing creep rate to-
rapidly for the aging at 649° C and above. The aging at 871° C ward a constant value is in evidence, and this creep rate remained
produced the lowest values at around 20 J beyond 10,000 h. For almost constant to beyond 15% strain. Investigators 关8,11兴 found
aging at 649° C and 760° C, the CVN energy values were near the that aging prior to creep eliminated the low creep rate at the start
minima after 1000 h. Figure 16 shows the CVN energy values of the test, hence the aged material creep at a high rate at the start
against the aging temperature for 1000 h of aging. It would appear of the test. In the study of Kihara et al., the 1000 h aged and virgin
that the decrease in CVN energy for some heats was less severe at sample eventually achieved the same creep rate. Schneider et al.
aging temperatures above 760° C, but this could be misleading if examined the effect of aging for times from 178 h to 8700 h.
further reductions occur beyond 1000 h, as shown by the data Again, the initial creep rate of the aged material was more rapid.
from Ref. 关14兴 in Fig. 15. A complete set of aging curves was Schneider et al. did not provide creep curves for comparison.
constructed by Bruch et al. that showed a 50% loss in the CVN Rather, they plotted the log creep rate against the creep strain. The
energy beyond 1000 h of aging at 700° C and 800° C. They ob- aged material appeared to follow a logarithmic creep trend, so it
served energy less than 10 J after 10,000 h of aging at 800° C and was possible to reconstruct the creep curves for comparison to the
900° C. The low CVN energy values for the long-time aging were curve for the as-annealed material. The reconstruction based on

Fig. 18 A creep curve for the annealed Alloy 617 at 950° C and 30 MPa; data source:
ORNL test

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Fig. 19 Reconstructed creep curve from Ref. †11‡ showing the effect of aging on the
early stages of creep at 950° C

the representation of primary creep, e, as a logarithmic function of are shown in Figs. 22–24. For the most part, the long-time aging
time t, is shown in Fig. 19, where e = a ln共1 + b · t兲. The curves had only a small effect on the continuous cycling fatigue lives. A
suggested that aging beyond a few hundred hours increased the few tests for a material aged for 10,000 h fell short of the general
initial creep rates. The curves tended to approach the “stable” trend at the lowest strain level, but the tests merit repetition before
creep rate observed for the annealed material. Most of the studies any conclusions could be drawn. Strizak et al. also found that the
on aging effects in creep were performed at a relatively high stress stress range at half life was not affected by aging at all three
and testing was generally limited to 2000 h or less. Some addi- temperatures. This observation differed from expectations based
tional testing was performed by McCoy and King 关14兴 but creep on the studies of tensile properties that found significant increases
curves were not provided and most of the testing was directed in strength for long-time aging at 704° C. An examination of the
toward the examination of aging in impure helium. The effect of cyclic stress-strain hysteresis loops did not reveal any significant
aging on the low-stress creep and on the rupture behavior remains
an unknown, but it is quite likely that aging effects will wash out.
However, several researchers observed that carbides redistributed
during the creep process. Under tensile creep, carbides were con-
centrated on boundaries normal to the tensile stress. There seems
to be a dependence on the magnitude of the stresses, as may be
seen in Figs. 20 and 21, that were obtained from the creep speci-
men used to produce the curve in Fig. 18. Figure 20 represents the
microstructure toward the shoulder of the sample and away from
the microcracking. Carbides are evenly distributed on boundaries
normal and parallel to the tensile stress. Figure 21 represents the
microstructure in a region where microcracking has developed.
Carbides were more massive and more often distributed on
boundaries normal to the tensile stress direction.

9 Aging Effects on Fatigue and Crack Growth


The investigations of long-time aging effects on the low-cycle
fatigue performed by Strizak et al. included aging at 10,000 h and
20,000 h at 538° C, 704° C, and 871° C 关13兴. Fatigue tests at
538° C indicated that aging at 538° C produced a small increase in
the fatigue life relative to the virgin material. Fatigue tests at the
aging temperatures of 704° C and 871° C produced lives that were
equivalent to or slightly less than unexposed material. The aging
for 10,000 h appeared to be more detrimental than the aging for Fig. 20 Microstructure away from the microcracking area
20,000 h. The relative loss in life was more severe at low strain showing the uniform distribution of grain boundary carbides
amplitudes and the aged life was half the virgin life. Plots com- after 881 h at 950° C „stress in the vertical direction…; source:
paring reported data on the fatigue response for three temperatures ORNL test

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damage may be significantly different if the carbides are oriented
on boundaries normal or parallel to the applied stress.
Very little is known about the effect of aging on the creep and
fatigue crack growth characteristics of Alloy 617. Since cracks are
usually linked to the surface of the specimen or component, it is
likely that the creep and the fatigue crack growth will be more
affected by the environment than the accumulated aging time.

10 Summary and Recommendations


This review identified a number of issues of importance regard-
ing aging phenomena in Alloy 617 that need to be addressed in
further experimental and analytical studies.
共1兲 Computational thermodynamics suggested that the equilib-
rium phases vary with temperature in the range of interest
to the VHTR. The critical temperatures and the weight per-
centages of the equilibrium phases depend on the composi-
tion within the specified chemical ranges for the alloy. Ad-
ditional studies are needed to further explore the variability
in the content of the equilibrium phases associated with Al,
Ti, C, N, and B for both the base metal and the filler metal.
Fig. 21 Microstructure in the microcracking area showing the 共2兲 The kinetics of precipitation of nonequilibrium phases ap-
preferential distribution of grain boundary carbides on bound- pear to vary from one set of experimental observations to
aries normal to the tensile stress „vertical direction…; source:
ORNL test
another. Investigations are needed to establish the processes
by which these phases are formed and replaced.
共3兲 Hardness data were found to be valuable in mapping the
kinetics of the property changes as a function of exposure
differences associated with aging, although the continued cycling history. Significant differences in the hardness values were
at higher strain ranges produced hardening and often suppressed observed from one heat to another with parallel exposures.
the dynamic strain aging that was present during the early cycling Explanations were not put forward. Hardness testing should
at 704° C and 871° C. Fatigue at low strain rates and with inter- be encouraged as a practical tool to accompany other types
spersed creep periods has been examined in other research activi- of materials evaluation that involve high-temperature expo-
ties in the US, Europe, and Japan but is outside the scope of this sures.
review on aging effects. One interesting aspect, however, deals 共4兲 The room temperature tensile yield and ultimate strengths
with the redistribution of grain boundary carbides observed under were increased by aging in the temperature range of
creep conditions. Creep-fatigue damage is often sensitive to the 600– 760° C. The rate of change in these properties was
grain microstructure so the compression and the tensile hold time temperature dependent and the maximum change varied

Fig. 22 Aging effect on the low-cycle fatigue at 538° C †13‡

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Fig. 23 Aging effect on the low-cycle fatigue at 704° C †13‡

with temperature and from one heat to another. The room temperatures. More experimental work should be planned
temperature ductility decreased as the aged strength in- to assess whether or not strength reduction factors will be
creased, and the ductility decreased after long aging times needed. These factors would relate to the “residual”
at temperatures above 760° C with no apparent minimum. strength at both high and low temperatures.
More research is needed to establish whether or not a duc- 共5兲 The fracture toughness, as measured by the Charpy V-notch
tility minimum could exist for very long times at VHTR energy, was greatly reduced by aging to long times. Values

Fig. 24 Aging effect on the low-cycle fatigue at 871° C †13‡

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ranged greatly from one investigation to another. For nearly nol., 66, pp. 289–295.
关12兴 Ennis, P. J., Mohr, K. P., and Schuster, H., 1984, “Effect of Carburizing Ser-
identical exposure conditions, energies ranged from less vice Environments on the Mechanical Properties of High-Temperature Al-
than 10 J to near 100 J. Further CVN testing is needed, loys,” Nucl. Technol., 66, pp. 363–368.
favorably in collaboration with research on radiation for 关13兴 Strizak, J. P., Brinkman, C. R., Booker, M. K., and Rittenhouse, P. L., 1982,
nuclear reactor applications. “The Influence of Temperature, Environment, and Thermal Aging on the Con-
共6兲 Short-time creep was affected by aging prior to testing. tinuous Cycle Fatigue Behavior of Hastelloy X and Inconel 617,” Oak Ridge
National Laboratory, Report No. ORNL/TM-8130.
Generally, aging increased the primary creep rate. Creep 关14兴 McCoy, H. E., and King, J. F., 1985, “Mechanical Properties of Inconel 617
tests on the aged material were typically 1000 h or less, and and 618,” Oak Ridge National Laboratory, Report No. ORNL/TM-9337.
the creep in the longer time tests tended to establish the 关15兴 McCoy, H. E., 1985, “Mechanical Properties of Hastelloy X and Inconel 617
same creep rate as the material that was not aged. However, After Aging 53,000 Hours in HTGR-He,” Oak Ridge National Laboratory,
Report No. ORNL/TM-9604.
short-time creep data are used as part of the construction of 关16兴 McCoy, H. E., 1986, “Evaluation of Advanced Alloys for Gas-Cooled Reac-
the isochronous stress versus strain curves. In design, these tors,” Oak Ridge National Laboratory, Report No. ORNL/TM-9891.
curves are used to estimate stress distributions following 关17兴 Garud, Y. S., 1986, “Development of a Physically Based Model for Material
short-time transients that can occur well into the lifetime of Strength and Embrittlement Under HTGR Operating Conditions,” S. Levy
Incorporated, SBIR, Report on Contract No. DE-AC03-85ER80219.
a structure. For this reason, further research to examine the 关18兴 Schubert, F., Breitbach, G., and Nickel, H., 1993, “German Structural Design
effect of aging on short-time creep and relaxation is justi- Rule KTA 3221 for Metallic HTR-Components,” High-Temperature Service
fied. and Time-Dependent Failure, ASME-International, New York, PVP-Vol. 262,
共7兲 Aging did not significantly affect the low-cycle fatigue be- pp. 9–18.
关19兴 Schubert, F., Nickel, H., and Breitbach, G., 1991, “Structural Design Criteria
havior at temperatures from 538° C to 871° C. However, for HTR–A Summary Report,” Nucl. Eng. Des., 132, pp. 75–84.
the testing was performed at the aging temperature, and the 关20兴 Corum, J. M., and Blass, J. J., 1991, “Rules for Design of Alloy 617 Nuclear
testing was of a short-time duration. Slower strain rate fa- Components to Very High Temperatures,” Fatigue, Fracture, and Risk, ASME-
tigue tests on aged materials are needed. An explanation is International, New York, PVP-Vol. 215, pp. 147–153.
关21兴 Srivastava, S. K., and Klarstrom, D. L., 1990, “The LCF Behavior of Several
needed for the lack of an aging effect on the fatigue
Solid Solution Strengthened Alloys Used for Gas Turbine Engines,” The Gas
strength and ductility coefficients. Turbine and Aeroengine Congress and Exposition, Brussels, Belgium, Jun.
共8兲 Models that incorporate aging effects into the creep process 11–14, Paper No. 90-GT-80.
were not treated in any detail in this review. However, the 关22兴 Lai, G. Y., 1993, “Nitridation of Several Combustor Alloys in a Simulated Gas
efforts of Garud 关17兴 that consider the influence of carbur- Turbine Combustion Environment,” Proceedings of the ASM 1993 Materials
Congress Materials Week ’93, Pittsburgh, PA, Oct. 17–21, pp. 113–121.
ization or decarburization need further consideration as to 关23兴 Meyer-Olbersleben, F., Kasik, N., Ilschner, B., and Rezai-Aria, F., 1999, “The
their applicability to aging effects. Also, the continuum Thermal Fatigue Behavior of Combustor Alloys IN 617 and HAYNES 230
damage models discussed by Dyson 关36兴 and Estrin 关37兴 Before and After Welding,” Metall. Mater. Trans. A, 30A, pp. 981–989.
need further consideration since they have the capability of 关24兴 Coade, R., and Tunjic, M., 2002, “Failure of an Inconel 617 Gas Turbine
Liner,” Proceedings of the Seventh Conference on Operating Pressure Equip-
incorporating changing metallurgical scenarios into the de- ment, Institute of Materials Engineering Ltd., Melbourne, Victoria, April 2–4,
formation and rupture processes. 2003, Vol. 7.
关25兴 Viswanathan, R., Purgert, R., and Rao, U., 2002, “Materials for Ultra-
Acknowledgment Supercritical Coal-Fired Power Plant Boilers,” Materials for Advanced Power
Engineering 2002, Forschungszentrum Julich GmbH, September 2002, pp.
This work was sponsored by the U.S. Department of Energy, 1109–1129.
Office of Nuclear Energy Science and Technology under Contract 关26兴 Swindeman, R. W., Shingledecker, J. P., Klueh, R. L., Wright, I. G., and
No. DE-AC05-00OR22725 with Oak Ridge National Laboratory, Maziasz, P. J., 2004, “Boiler Materials for Ultra Supercritical Coal Power
Plants Task 2: An Assessment of Candidate Materials–A Review of Literature
managed by UT-Battelle, LLC. Part I: Overview and Recommendations,” National Energy Technology Labo-
ratory, Report No. NETL/DOE, USC T-7.
关27兴 Starr, F., and Shibli, I. A., 2000, “Fundamental Issues in the Development of
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