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Fusion Engineering and Design 36 (1997) 251-267

ELSEVIER

Fusion Engi ng aridDesmgn

Fracture mechanics behavior of a N i - F e superalloy sheath for superconducting fusion magnets. Part 1. property measurements 1
R . L . T o b l e r a,,, I.S. H w a n g u, M . M . Steeves c
a National Institute of Standards and Technology, Boulder, CO 80303, USA b Seoul National University, Seoul 151-742, South Korea c Massachusetts Institute o f Technology, Cambridge, MA 02139, USA

Received 8 July 1996

Abstract

A seamless extruded conduit for superconductor cabling was fabricated and subjected to mechanical tests. The conduit is made of a nickel-iron alloy having aging and thermal contraction characteristics comparable with Nb3Sn conductors. The conduit in liquid helium at 4 K retains its ductility and offers high strength, toughness, and fatigue resistance. Specimens with surface cracks in tension offer substantial fracture resistance for the practical case of crack propagation in the through-wall direction. Fatigue tests indicate that surface cracks adopt a nearly semicircular shape as they grow through the conduit wall (L-S orientation) at rates in the power-law region that are no faster than rates in the transverse direction (L-T orientation). The serviceability of this material is discussed.

1. Introduction

A nickel-iron superalloy (Incoloy 908) 2 was recently developed for use in fusion magnets as a sheath for cable-in-conduit superconductors [13]. A sheath is a tubular load-bearing member

* Corresponding author. Contribution of NIST. 2 Tradenames are used herein for material identification only and do not imply endorsement of the products or manufacturers by the authors or by NIST. Other materials by other manufacturers may work as well or better.

that supports Nb3Sn superconductors while carrying supercritical helium at 4 K. F o r such applications the superalloy offers potential benefits. Unlike austenitic stainless steels, the superalloy is not degraded by heat treatments typical for Nb3Sn fabrication. Its thermal contraction below 1000 K is compatible with Nb3Sn, so compressive strains imposed on superconductors during cooling are optimized. A sheath must withstand high static and cyclic stresses arising f r o m L o r e n t z forces at temperatures as low as 4 K and in magnetic fields as high as 14 T. The fatigue properties o f the sheath alloy

0920-3796/97/$17.00 1997 Published by Elsevier Science S.A. All rights reserved.


PIIS0920-3796(96)00701-6

252

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

will often limit the design life of an advanced fusion system [4]. Mechanical failure of the sheath or helium leakage are both unacceptable since replacement or repair is prohibitively expensive. Flaw inspection is also problematic. Therefore, the structural reliability of magnets is a primary design requirement in advanced devices such as the International Thermonuclear Experimental Reactor. Fracture mechanics behavior under the circumstances is critical to material selection. Relevant data for the Ni-Fe superalloy are promising, but limited to developmental heats of material in the form of wrought plates [1-3,5-8]. We report new measurements here, extending the database to commercially fabricated tube products.

2. Experimental procedure
We obtained a seamless extruded conduit (SEC) [5] and conducted tension, fatigue, and toughness tests in ambient air (295 K), liquid nitrogen (76 K), and liquid helium (4 K). Surface-cracked tension (SCT) tests were used to evaluate crack tolerance in the through-wall direction at 4 K. SCT tests are described in ASTM Practice E 740. By definition the crack depth is a, the total crack length is 2c, and the aspect ratio is a/c. The quantities determined in SCT tests include the growth rates of fatigue cracks and residual strengths for specimens with part-through cracks on one surface. The residual strength of a cracked specimen is a function of test temperature, crack dimensions, and specimen thickness; it reflects the maximum load that can be sustained, and is particularly meaningful for conduits where crack propagation through the wall is a likely mode of failure in service.

product was rectangular, with external dimensions of 38 by 52 mm and a wall thickness of 6,7 mm. The nominal grain diameter was 74 gm and the Vickers hardness was 295 kg mm 2. Ten pieces of conduit 250 mm long were obtained for testing. Each piece had residual cold work ranging from 8-14%. Specimens were taken from strips representing the broad sides of the conduit. The specimens were machined out, heat treated, and tested in that order. Fig. 1 shows the sequence of operations involved in specimen manufacture. Fig. 2 shows the layout and relative orientation of the conduit strips and blanks used to make the three types of pin-loaded test specimens. Tensile specimens had a longitudinal orientation, a gage length of 30.5 mm, and a 6.2 x 4.6 mm cross section. Compact specimens were 6.2 mm thick and 35.5 mm wide, with standard planar proportions and clip gage retention points located at the specimen edge or loadline. The compact specimen geometry is diagrammed elsewhere [8], and according to ASTM standard notation its fracture plane orientation is L-T.

1"~----52.5m m - - ~

r rail l ~

255mm

~I

2.1. Materh~l and test specimens


The SEC was obtained from a commercial manufacturer and tested in the aged condition (923 K, 200 h). The chemical composition in mass percent is: 49.42Ni-40.80Fe-3.99Cr-2.94Nb-1.55Ti- 1.03A10.16Si-0.04Mn-0.01C-0.01Cu-0.01Mo-0.01Co-0.01 Ta-0.004P-0.003B-0.001S. The material was extruded, tube-reduced, and hydrogen-annealed in a series of steps outlined previously [5]. The final

I HeatT~m~t (~O'Cf~ 2~ h i~~c~uml I Fig. 1. Sequence of operations for specimen manufacture.

,l

R.L. Tobler et al. /Fusion Engineering and Design 36 (1997) 251-267


I~

253
-*q

Tensile Tensile

#1

#2

Compact

38.1

I~ ,si,,.
=45x 43 mm

38x 126mm

size : 26x 82 mm 0

Blank

Blank size

Compact

#T~'nsion

Tensile Tensile

#3

#4

0
Compact
.

#T~lsion

! Flaw #2

Surface

0
Compact Ten,~on #4

I
l 6_.21
t

0
Compact Tension

#5

Fig. 3. Surface-cracked tension specimen. Fig. 2. Plan for specimen cutting, showing how specimen blanks are sized and oriented in three 250 mm strips from the broad sides of conduit. Fig. 3 shows the SCT specimen geometry. Its width (W) is 12.5 m m and its reduced-section length is 50.8 mm. Eight specimens were roughmachined, heat treated, final-machined, and mechanically polished to a final thickness (B) of 6.2 mm. This thickness is essentially equal to the wall thickness of a conduit in service. Heat treatment was performed in vacuum (0.00133 Pa) at 923 K for 200 h, followed by furnace cooling. Electrodischarge machining ( E D M ) produced the slit sizes shown in Table 1. Four of the specimens had semicircular slits, and four had semielliptic slits. The slits were 0.09 4-0.02 m m wide and centered on a broad side of the reduced section in the L-S Table 1 Nominal starting flaw sizes for SCT specimens Flaw shape Semicircular Semielliptic a (mm) 0.889 0.127 2c (mm) 1.778 2.540 orientation. The tensile axis is therefore parallel to the extrusion direction, and cracks in the SCT specimens travel in a direction through the conduit wall.

2.2 Strength and fracture toughness


A S T M procedures were followed for tension tests (Methods E 8-94a and E 1450-92) and toughness tests (Methods E 399-90 and E 813-89). In ductile fracture tests, a J-resistance curve (plot of J vs. crack extension) is determined. A quantitative measure of ductile fracture toughness J~c is then operationally defined as the point of intersection of the resistance curve regression line and a blunting line, J=2~rvAa, drawn at a 0.2 m m offset (ASTM E 813-89). A corresponding fracture toughness value in terms of the linear elastic parameter K~c is estimated from (E x j~)l,.2, where E is Young's modulus.

a/c ( - )
1.0 0.1

2.3. Fatigue crack initiation and growth


Fatigue crack initiation at notch tips having a radius p was studied using compact specimens.

254

R.L. Tobler et al. / Fusion Engineering and Design 36 (1997) 251-267

The number of cycles required to initiate a 0.25 mm fatigue crack is defined as the crack-initiation life Ni and correlates with AK/x/p, a parameter proportional to the change in maximum elastic stress at the notch root. We assume that Ne depends on the maximum elastic stress Smax ahead of the notch and that Smax is proportional to K/x/p, where K is the applied nominal stress intensity factor [9,10]. The nominal value of K is calculated from expressions for the standard stress intensity, using the notch length as if it were equivalent to a sharp crack of length a [10]. Cracking was detected from changes in the load-displacement slope as the specimens were cyclically loaded at a stress ratio R = Pmin/Prnax (minimum load/maximum load) = 0.1. During periodic interruptions for single-cycle loadings, the load-displacement data were fed to a computer for real-time data reduction, and a standard compliance function was used to infer the instantaneous crack length as a function of load cycles N. The resulting plots of a-vs-N were analyzed for crack initiation and growth. Ne was determined at Aai= 0.254 mm and plotted vs. AK/x/p, where AK is Kr~x - K~n for the fatigue load cycle. The growth rates da/dN of fatigue cracks were calculated using short-crack simulation (SCS) and constant-stress-ratio techniques. The conventional test maintains R = 0.1 and is used at moderate or high AK values. The SCS test maintains the maximum stress intensity factor Kmaxconstant while R gradually increases from 0.1-0.7. The SCS approach is used at low AK (below 25 MPa x x/m) to efficiently generate a conservative threshold stress-intensity factor AK-rh. We used these techniques before, and elsewhere describe the fatigue apparatus and test procedures in more detail [7121.

Specimens with semicircular slits (a/c = 1) were fatigued in axial tension using maximum fatigue loads equal to 30 or 40% of the ultimate tensile strength at 295 K. Precracks formed in 111 000 cycles or less, and the final a/c ratios varied between 0.87 and 0.97. One specimen with an elliptical slit (a/c = 0.1) was fatigued in tension, but cracks formed at the loading-pin holes as well as at the EDM site. To prevent this, the other specimens having elliptical slits were fatigued in 3-point bending using a table-model 100 kN servohydraulic machine and a bend-test fixture with roller pins adjusted to a span of 63.5 mm. Rates of fatigue crack growth in the L-S orientation (295 K) were calculated for two SCT specimens. The 2c-vs.-N data obtained during precracking were used to estimate da/dN values for cracks moving in the wall thickness direction. In this estimation, the flaw aspect ratios were interpolated between the initial EDM value Eq. (1) and the final values (measured on the fracture surfaces) following Newman and Raju's method [14]. After precracking was completed, each SCT specimen was cooled to 4 K and fractured in a single loading using a 250 kN servohydraulic machine in displacement control. The loading rate to fracture was within the normal range used in standard 4-K tension tests, and time to fracture was about 5 min. The load-stroke curves were recorded, and residual strength was calculated from the maximum load at fracture divided by the specimen's original cross-sectional area (Method E 740, section 7.6).

3. Results

3.1. Tensile and fracture toughness properties 2.4. Surface crack tension tests
The SCT specimens were fatigue precracked at 295 K and then fractured under uniaxial tensile loading at 4 K. the fatigue loading at 10 Hz and R = 0.1 was periodically interrupted to measure the crack length 2c by an optical method. Precracks of various shapes and sizes were created by fatigue in axial tension or three-point bending [13]. Table 2 presents the tensile test results. The tensile strength and ductility parameters for this material are mildly temperature dependent. The behavior resembles that of other aged superalloys [15-18] in showing a moderate increase of yield strength, a larger increase of tensile strength, and significant ductility at temperatures between 295 and 4 K. The average value of the yield strength

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251 267

255

Table 2 Results of uniaxial tension tests at three temperatures. Temperature(K) 295 Average 76 Average 4 Average YS (MPa) 1020 980 990 997 1135 1070 1102 1120 1190 1155 UTS (MPa) 1270 1250 1240 1253 1540 1540 1540 1635 1680 1658 EL (%) 22 22 19 21 25 29 33 22 26 24 RA (%) 38 35 37 37 40 39 38 28 32 30

at 4 K is 1155 MPa, near the targeted value of 1200 MPa [2]. Table 3 lists the fracture toughness measurements and related parameters at 295, 76 and 4 K. Linear elastic procedures (Method E 399) produced KQ data as shown, but valid KIo data could not be obtained directly, due to substantial plastic deformation in the 6.2 mm specimen thickness. We applied elastic-plastic procedures (Method E 813-89) instead. Fig. 4 and Fig. 5 show a typical resistance curve and the specimen fractured in that test at 4 K. As shown in Table 3, the critical J values and corresponding Kic estimates derived from them are mildly temperature dependent and increase modestly with temperature reduction between 295 and 4 K. The average Kic estimate (196 MPa x x/m) at 4 K virtually equals the targeted value of 200 MPa x/m. Fig. 5 is representative of the failed compact specimens which were similar in appearance regardless of test temperature. The zone of highest reflectivity and brightness corresponds to the fatigue crack. Above that is located the fracture surface created during the J-test, which consists of a zone of fiat fracture, bordered on both sides by shear lips which are cusps projecting out of the plane of the photograph. The fiat-fracture zone is trapezoidal since the shear lips increase in size as fracture progresses. Scanning electron mi-

croscopy at higher magnifications revealed dimples on all the fracture-zone surfaces, confirming the existence of a ductile failure mechanism at each test temperature. The dimples for compact specimens are similar in appearance to those for the SCT specimens shown later in the text. The critical J measurements in this study are denoted JQ (not J~) because the standard requirements regarding uniform crack advance beyond the fatigue crack front could not be satisfied in these tests. As illustrated in Fig. 5 for the representative specimen, fatigue precracking always produced satisfactory crack-front straightness, but quasistatic loading to fracture caused preferential crack advance at the center of specimen thickness (tunnelling). Owing to tunnelling, the requirements for ASTM E 813-89 paragraph 8.4.3.10 cannot be satisfied, and close agreement between the final physical crack size and the compliance-predicted crack size according to paragraph 9.4.1.7 was lost. Some implications and mitigating factors are noted later in the Discussion.
3.2. Fatigue crack initiation

Data for fatigue crack initiation are plotted in Fig. 6. The number of cycles needed to generate a fatigue crack increases at cryogenic temperatures, especially between 76 and 4 K. For all tempera-

256

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251 267

Table 3 Results of toughness tests at three temperatures Temperature (K)


295

Thickness (mm)
6.044 6.222 6.172 6.274 6.324 6.222 6.122

Width (mm)
35.560 35.510 35.510 35.560 35.510 35.560 35.510

a/W ( - )

Pmax/PQ(--)

KQ (MPa x x/m) 170a 100 113 117 125 124 102

JQ (kJ/m 2) NA NA 165 215 227 221 210 201 205

Ktc(J) (MPa x x/m) NA NA 171 200 206 203 198 193 196

0.614 0.589 0.592 0.591 0.601 0.600 0.585

1.02a 1.56 1.42 1.62 1.46 1.52 1.80

76

Average
4

Average aAccidental overload occurred in this test. For discussion of test validity requirements, see text.

tures and stress ranges considered in our experiments, a power-law expression applies:

3.3. Fatigue crack growth


Fig. 7 shows measurements of da/dN for the L-T oriented compact specimens at 295 K. Cracking rates at R = 0.1 for the SEC were obtained in the range 15 < A K < 50 MPa x x/m. Also in this figure is a band representing previous SCS data

Ui = A ( A K / x / p ) -b

(1)

where A and b are empirical constants. As shown in the figure, data conforming to Eq. (1) display linear trends when is plotted vs N,. using log-log coordinates. For such plots, A is the intercept on the ordinate axis at N i = 1, and - b corresponds to the slope of the straight line. For the trendlines shown in Fig. 6, Table 4 lists the empirically determined values of A and - b at each test temperature.

AK/x/p

80C

70 60 '~
500

Alloy 908 T=4K

20C

10C

0.5

1.0
Crack Extension, Aa, mm

1.~

Fig. 4. J-resistance curve for compact specimen at 4 K.

Fig. 5. Compact specimen fractured at 4 K.

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

257

500(3
Q.

4K

Compact Specimen

295 K ~
~b~..~. ~.~-~"

1000

B --621 m m W = 35.6 mm an = 1 4 . 5 m m p = 0.077 mm

500
5 10'* s 10 5

Number of Cycles to Initiate 0.25 rnnrnCrack

Fig. 6. Cryogenic effects on fatigue crack initiation life.

for wrought plates beginning at A K = 30 MPa x x / m (R = 0.1) and ending at A K = 2 MPa x x / m (R < 0.7) [8]. the plate and conduit results agree at A K = 20-25 MPa x x/m, where R = 0.1 or nearly 0.1 in both types of tests. Below A K = 2 MPa x x/m, divergence appears in the form of a kink or knee in the trendline for the conventional (constant R-ratio) results o f this study. Fig. 8 shows measurements of da/dN obtained at 76 K. Again, conventional data for the SEC of this study (R = 0.1) are compared with earlier SCS data for wrought plates (variable R). The data at R = 0.1 extend to rates as low as 10-6 mm per cycle. Extrapolating the trend to 10 - 7 m m per cycle indicates a threshold of about 8 MPa x x / m at this temperature, whereas the SCS results indicate a much lower threshold: AKTh = 3.5 MPa x x/m. Presumably, 3.5 MPa x ~/m is the intrinsic threshold and 8 MPa x , J m is an apparent threshold affected by the test procedure at R = 0.1. In another study of annealed 316 L N steel, a similar difference in threshold values was reported, and crack closure at R = 0.1 proved to be the cause of the higher threshold in conventional tests [8,11]. Fig. 9 shows the measurements of daMN obtained at 4 K. In this study, we obtained SCS data for the SEC at AK below 25 MPa x x/m, and conventional data (R = 0.1) in the range 17 < A K < 100 MPa x/m. The SCS trend shows a sharp knee at A K = 13-15 MPa x x / m that is more pronounced than the knees at 76 or 295 K. Below z l K = 20 MPa x x / m the conventional and SCS trendlines diverge as R begins to increase in the SCS tests. Thus, the SCS results of this study

give a relatively high threshold, d K x h = 9 - 1 0 MPa x x/m, which repeats and confirms earlier findings for wrought plates [8]. Regarding behavior at the opposite end of the curves for da/dN vs. AK, at very high AK values, the cracking rates at 76 and 4 K do not show drastic increases as displayed in some other materials. In the tests at R = 0 . 1 we increased the maximum fatigue loads until Kmax was equal to the KQ values applied in fracture toughness tests at these temperatures. Nevertheless, Fig. 8 and Fig. 9 show no departures from the midrange trends, which implies no unstable cracking at high AK. Instead, the growth rates of fatigue cracks at AK up to 100 MPa z x / m simply continue along the same trendlines that apply in the midrange of the da/dN curves. The well known law for midrange behavior is da/dN = C(AK)" (2)

where n is an exponent and C is the value of da/dN at A K - - 1. For our purposes, good empirical fits to this law are obtained with n fixed and equal to 3 at any temperature. Considering da/dN in the range 3 x 1 0 - 4 - 1 x 10 - 3 and using n = 3 , the value of C decreases progressively with temperature as shown in the Table 4. Therefore, at intermediate A K values, the resistance to fatigue crack growth increases at cryogenic temperatures owing to the temperature dependence of the coefficient C. Fig. 10 compares da/dN measurements obtained using the two different specimen geometries. In the previous figures, only data from compact specimens have been shown. Here, data at room temperature for SCT (L-S orientation) and compact specimens (L-T orientation) are compared at 15 < A K < 30 MPa x x / m (that is, in the limited range covered during the SCT precracking stages). The results for these two orientations agree within a factor of 2, which is within the typical range of error for daMN data. Regression-calculated fits using Eq. (2) for the data from SCT specimens produced essentially the same exponent (n = 2.97) as found for the compact specimens, and the L-T data trendline falls near the upper bound of the scatterband for the L-S data. Therefore, the cracking rates of this extruded and heat-treated conduit can be considered isotropic for the range of A K considered.

258

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

Table 4 Fatigue equation parameters for initiation and growth of cracks Specimen type Test temp. (K) Fatigue crack initiation, Eq. (1) Coefficient, A (MPa) Compact
295 76 4 295 1.0 x 1016 9.9 x 1016 3.8 x 1019 NA

Fatigue crack growth rate, Eq. (2) Coefficient,


C (mm/cycle) 5,00 x 10 -9 4.25 x 10 -9 2,40 x 10 -9 2,69 x 10-9

Exponent,
- b (-) 3.4 3.6 4.2 NA

Exponent,
n (-)

3 3 3
2.97

SCT

3.4. Surface crack tension tests

Table 5 lists the SCT test parameters and resuits. The patterns of crack growth, residual strengths at 4 K, and fractographic results are discussed below. The initial dimensions of the EDM flaws and surface cracks changed during fatigue, as shown in Fig. 11 and Fig. 12. These figures show the original EDM slit sizes plotted along with the final dimensions of surface cracks measured from the fracture surfaces of broken specimens.
AK
10 -2 , , i I lll~l 0 5O 100

For semicircular EDM flaws in axial tension (Fig. 11 and Fig. 12), after any increment of fatigue crack propagation the aspect ratio drops below the starting value of 1 and assumes slightly lower values near 0.9. But for semielliptic EDM flaws (a/c = 0.1) in 3-point bending (Fig. 11), the aspect ratio depends on the extent of crack growth; for a few specimens tested in this study, the aspect ratio increases significantly from the starting value of 0.1 and adopts values in the range 0.58-0.74. Regarding the growth of these semielliptic cracks, longer crack extensions consistently produce larger aspect ratios.
z~K
--10,2 I 10 I I I Illrl I 50 100 ~ I I I1111 I T=76K

T=295K

10-3 10 -3 !:

E
Z

10 "4
10 .4

"1o
e-

l O "~

Plata=,

///.~

Conduit, 11
:~ 10 .5

Plates,

10 "~

V
~10-6

10-7 /~/i i illlll i i i llllll I


2 5 10 20 50 100

10 .7

Range of K, MPa. , ~
Fig. 7. Growth rates of fatigue cracks at 295 K,

10

20

50

100

Range of AK, MPa. ,/~


Fig. 8. Growth rates of fatigue cracks at 76 K.

Table 5 SCT specimen size, fatigue loading, final crack size, and 4-K residual strength a~ EDM flaw 1.0 1.0 1.0 1.0 0.1 0.1 0.1 0.I T, T, T, T, T, T, B, B, 35.6 26.7 29.8 26.7 35.6 35.6 3.0 3.0 10 90 55 111 40 71 80 60 1.218 1.396 1.854 2.996 NA 0.864 1.320 1.778 2.514 3.150 4.266 6.552 NA 2.972 4.038 4.826 0.97 0.89 0.87 0.91 NA 0.58 0.65 0.74 Fatigue loading~ Cycles ( 100) a (mm) 2c (mm)

Spec. No

B (ram)

W (ram)

a/c ( - )

emax (kN) 123 120 116 99 NA 108 127 126

6~ @ 4 K (MPa) 1720 1620 1460 1240 NA NA b 1570 1620

201 202 203 204 205 208 206 207

5.850 5.800 6.275 6.250 6.225 5.925 6.350 6.150

12.295 12.725 12.700 12.700 12.675 12.675 12.700 12.675

aT is axial tension, B is 3-pt bending, and maximum fatigue load is shown in kN. bThe residual strength measured at 295 K is 1460 kN.

260

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267


AK 10 F ,lllll i i T=4K 4--50 100 i ~1111 q q

I
0.6

10 .2

m ."
3

0.5
S~a~i~L_rcular

10 .3

o~ E E

S'
S.~ Conduit, R:0.1 10 -4

E E
J= a (3

I d e a l l y ! ~

0.4 0.3 ~. 0.2


0.1 (3

Z 03 nr
_he

Plates,
Variable , ~ / ~ . , : 10 "s

(3

Slit I
1

==

L 2

[ 3

;0

:e 10"s

Crack Half-Length c, mm

LL

Fig. 11. Changes in flaw dimensions after axial fatigue.

~ 2 = 1 -I- 1.464(a/c) 165


10 .7
.... , ,

(3)

10 20

50 100

Range of AK, MPa.,/~

Fig. 9. Growth rates of fatigue cracks at 4 K.

For specimens with nearly semicircular cracks, Fig. 13 and 14 plot the residual strength ar vs. various crack size parameters. For these specimens, the measured final a/c ratios ranged between 0.87 and 0.97. The residual strength at 4 K ranges from 1725 to 1245 MPa, decreasing nonlinearly with crack size according to the trend in Fig. 13. Fig. 14 shows the residual strengths as a function of two relative crack size factors, a/B and a/~ 2, where
10<

Apparently both parameters give nearly linear trends for medium-sized cracks, but the linearity is lost for larger cracks (a/B > 0.3 or a/~2> 0.9). The residual strengths at 4 K for three specimens with semielliptic cracks are also shown in Fig. 13. For these, the final aspect ratios range between 0.58 and 0.74. The data are too few to define a trend, but for similar values of 2c the semielliptic cracks give higher residual strengths than semicircular cracks simply because the
i i i i I i ~ =

AxialTension Fatigue
E E

I Compact Specimen

i
i

.."

(L-T)

2
~>, 10 ~

o~

Bending

~ e r
Fatigue

~
SlitSizes . ~ . . . . ~

(3

E E

Z
--~ 10 -~

ct)

0"10

20

30

40

50

AK (MPa. 4ff'i)

0.5

1.0

Aspect Ratio a/c

Fig. 10. Room temperature da/dN data from compact and SCT specimens,

Fig. 12. Flaw dimension changes in 3-point bending and in tension.

R.L. Tobler et a l . / Fusion Engineering and Design 36 (1997) 251-267


1817o -

261

0 7 " Nearly Semicircular Crack, T = 4 K " ~ (a/c. 0.9 ) ~:~ 1600 ~ ) O3 "~ 1400 o ~ Semielliptic Cracks, T = 4 K ~ " ~ , ~ (a/c = 0.85, 0.74) 125

g
w

1200

I
4

I
5

I
6

Z .; O --I

C r a c k Length

2c,

mm

Fig. 13. Residual strength vs. crack length.

semielliptic cracks are shallower. Just one specimen with a semielliptic crack ( a / c = 0 . 5 8 ) was tested at 295 K; as expected, it produced a somewhat lower residual strength compared to the specimens tested at 4 K. Fig. 15 is a representative fracture test record for an SCT specimen. All test records at 4 K were nonlinear and finely serrated, which are qualitative indications of ductility. Other indicators demonstrating material ductility despite the existence of surface cracks are shown in Fig. 16. As in conventional tension tests of unflawed specimens, we calculated a 'residual reduction of area' RA for the SCT specimens by piecing the broken specimen halves back together, measuring the final dimensions at the neck, and calculating the per cent change relative to the original cross sectional area: (Ai - Ar)/Ai x 100 = RA. Similarly, we take the stroke travel required to fracture a specimen as a measure of the speciParameter a]~

I
7

Displacement,

mm

Fig. 15. Load-vs.-stroke displacement for an SCT specimen at 4K.

men's ability to elongate during tensile load application. A brittle material will naturally show low values of stroke travel, as well as low values of residual RA without much effect due to crack
81
I I I I
3

Semicircular Cracks

7 E E ,c" 15
o

T=4K

11

1800 0]2

0.4
I

0.16

0.8
l

1.0
I

1.2
j

1,4

lO r
,<

:
1so0

4
3

9 ,5

.g_
==
O
2
7

14o~

1 no 1200 ~ ~ 0.2 0,3 t 0,4


I 0.5

C r a c k Length 2c, m m

Relative C r a c k Depth a/B

Fig. 14, Residual strength vs. relative crack depth.

Fig. 16. Stroke displacement to cause fracture and residual ductility of SCT specimens tested at 4 K.

262

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

Fig. 17. Specimen 203:4.5 x view of the reduced section after fracture at 4 K, showing front face with surface crack (right) and back face (left). size. I n c o n t r a d i s t i n c t i o n , the findings for o u r S C T specimens with semicircular cracks in Fig. 16 feature significant values o f residual ductility a n d the s t r o k e travel to fracture at 4 K. B o t h p a r a m e ters are sensitive to, a n d inversely related to, c r a c k size.
3.5. Fractography

F r a c t o g r a p h s in Figs. 1 7 - 2 2 are r e p r e s e n t a t i v e for S C T specimens with n e a r l y semicircular c r a c k s t h a t were tested at 4 K. Fig. 17 shows front a n d b a c k views o f specimen

Fig. 18. Specimen 203:6.5 x view, normal to the fracture plane.

Fig. 19. Specimen 201: SEM overview at 33 , showing: the EDM flaw, the 295-K fatigue crack, and the fracture surface formed at 4 K.

R.L. Tobler et al./Fusion Engineer&g and Design 36 (1997) 251-267

263

Fig. 20. Specimen 201:500 view of the EDM slit surface. 203 (a = 1.854 mm, 2c = 4.266 mm) after deformation and fracture in liquid helium. The front view shows the horizontal surface crack and two 45 slant fractures in the ligaments at both sides. Localized deformation is indicated by the necked ligaments. Uniform deformation before necking and fracture is indicated by the 'orange-peel' effect which appears everywhere on the specimen's reduced section except in the stress-free locations just above and below the surface crack (these undeformed areas retain their original polish). Fig. 18 views specimen 201 ( a = 1.218 mm, 2c = 2.514 mm), normal to the fracture plane. The semicircular E D M flaw is surrounded by a more reflective crescent-shaped fatigue crack produced by axial loading at R = 0.1. The flat-fracture zone is trapezoidal, and surrounded on three sides by

Fig. 22. Specimen201:750 x view of the 4 K fracture surface. shear lips produced by fracture surfaces slanted at 45 to the fatigue crack plane. Apparently, stable flat-fracture propagates to a depth of 4 mm (about 65% of thickness) before unstable failure occurs. Fig. 19 is an SEM view of the same specimen, showing the semicircular E D M flaw, the crescentshaped fatigue crack formed at 295 K, and the fracture zone formed at 4 K. Enlarged images are shown in Figs. 20-22. Fig. 21 reveals crystallographic facetting with some secondary cracking on the fatigue surface at 295 K. Fig. 22 shows a network of dimples and microvoids on the overload fracture surface which confirms again that a ductile failure mechanism is retained at 4 K.

4. Discussion
4.1. Material comparisons

Fig. 21. Specimen 201:500 x view of the 295 K fatigue.

The tensile and toughness properties of the conduit are mildly temperature dependent, and cryogenic effects are favourable. Toughness variations with temperature for selected superalloys [15-19] are compared in Fig. 23. Included are two heats of alloy 718 [15,18], representing different processing histories. Such data are sufficient to demonstrate that the Ni-Fe superalloy of this study behaves qualitatively like other precipitation-hardened superalloys of its class. The strength-toughness combination of the conduit material at 4 K is also attractive. This is

264
1.4 i

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267


I

1.3
iAlIoy 1.2 ~ _~_ ~ ~ 908 / A l l o y 71 El /AUoy766 Alloy 718

~t.t

1.0.................................... 0 . 9 ~ o y 6.8 0.7,1 0


100

750

200

306

Test Temperature, K

Fig. 23. Cryogenic effects on the toughness of superalloys.

shown in Fig. 24, where austenitic stainless steels are represented by a trendline for commercial 304-type steels having the T-L fracture plane orientation. The conduit specimens of this study had the L-T orientation, whereas the plate specimens in a previous study were T-L [8].
4.2. Fracture test validity

Although our results do not satisfy all the requirements of the standard J-test, ASTM Method E 813-89, nevertheless it can be argued that the data retain significance for the purposes in view. Standard test criteria are intended to assure that test results will be size-independent and reproducible, whereas we have practically nullified size effects by testing a specimen that is identical in

400
3o0

i T=4K

:E
20C

Alloy 908,

receivedplate
Alloy 908,

==
03

ged conduit
i Alloy 908,

16(
o
400

aged plate

8;0

1200

'

t6;o

2000

Yield Strength, MPa

Fig. 24. Strength-toughness combinations at 4 K.

thickness to the part that will be placed in service. The design-relevance of the fracture toughness data is thereby bolstered considerably. As mentioned previously, the main problem in standard J-tests of the 6.2 mm compact specimens of is that crack extension at the center of thickness outdistances crack extension at specimen edges where sizable shear lips formed. The requirement of section 8.4.3.10 of the J-test standard is violated because the individual crack length measurements deviate from the ASTM average crack length by much more than 7%. As a consequence, the compliance-predicted final crack extensions in our J-tests are about 25% shorter than the physically measured crack extensions, whereas the disparity should not exceed 15% according to Section 9.4.1.7. The effects of tunnelling are most severe at the end of a test. The reason is that disparities between the ASTM average crack length and the individually measured crack lengths near the specimen edges progressively increase as the shear lips are enlarged during the course of the test. Judging from Fig. 5, shear lips ultimately occupy 60% of the overall specimen thickness while the intervening flat-fracture zone diminishes in proportion to about 40%. The fidelity of the compliance-predicted crack lengths is compromised since, in contradistinction to the assumptions of compliance analyses, a considerable portion of material fails by a process of slant fracture occurring out-ofplane and lagging behind the flat-fracture front. Conversely, the effects of tunnelling are less pronounced at the beginning of the fracture test, where the critical J value is determined. As shown in Fig. 5, fatigue crack fronts in compact specimens of the superaUoy are quite straight and fully acceptable. The minimum crack length measurement at the specimen edge typically deviates from the ASTM average length by - 3 % , whereas the maximum crack length at mid-thickness deviates by + 1%, and deviations up to 7% for both are allowed by the standard. As a result, the initial crack lengths are accurately inferred by compliance with uncertainty of less than 1%. Similarly, the critical J values reported in this study are not subject to gross error since they are derived using an offset procedure applied to the early part of the resistance curve at Aa = 0.2 mm.

R.L. Tobler et al./ Fusion Engineering and Design 36 (1997) 251-267


100 , , i I

265

,
Min

--

-/

Size Required for Val d KIc Test / (ASTM E 399)

E E

2O

1 ........ s_i_z?_te_s_t _ed__in_this- _stu_d_y_R . . . . . . . . . . . . . . .

g
E

Min. Size Required for Valid Jle Test / (ASTM E 813)

i 4 ~ ;~6

295

Test Temperature, K

Fig. 25. Thickness requirementsfor valid toughnesstests, and conduit specimen thicknessof this study. Regarding size effects, Fig. 25 projects the minimum thicknesses required for valid toughness tests. The thickness required for J-tests is calculated from Method E 813-89, section 9.4.1. The thickness required for linear elastic response and valid Kic measurement is calculated from Method E 399-90, section 9.1.3, using the Kit(J) estimates (Table 2). For our 6.2 mm compact specimens, the J-test size criterion is satisfied at all test temperatures whereas the linear elastic size criterion is satisfied at none. The outcome is favourable in that an elastic-plastic response in service is preferable to a linear elastic one. The calculations are of further interest in giving some indication of the material response that may be expected in future applications. Based on these data, linear elastic fractures would be unlikely in service components at 4 K unless the alloy were used in section thickness more than 10 times greater than the conduit wall thickness tested in this study.
4.3. Residual strength

according to Practice E 740. In liquid helium, the SCT specimens fracture before stable cracking can fully penetrate the wall. Appreciable ductile fracture resistance is indicated by all criteria of performance. Nonlinear loading is associated with plastic deformation and concomitant slow crack growth, followed by unstable fracture and shearing of ligaments on three sides of the test section. As shown in the text, the residual strength at 4 K decreases regularly with flaw size, ranging from 1720-1425 MPa for crack lengths 2c ranging between 2.5 and 6.5 mm (nearly semicircular cracks). The 1720 MPa value is actually 5% higher than the average ultimate strength (1658 MPa, Table 2) measured in conventional flaw-free tension tests. Thus, there is some material inconsistency for the two specimen types, even though the same nominal stock and heat-treating conditions were used. Scatter in strength measurements can arise from variations of cold work in the specimen strips before aging. Or, the inconsistency may inadvertently derive from a difference in thermal response, since the SCT specimens and conventional tension test specimens were heattreated in two separate batches on separate occasions.
4.4. Fatigue resistance

The fatigue resistance of the conduit improves at cryogenic temperatures, and some fatigue parameters described below show greater improvement between 76 and 4 K than between 295 and 76 K.
4.4.1. Fatigue crack initiation Crack initiation behavior resembles conventional fatigue life behavior in that: (1) the 3 K / x/p-vs.-N~ curves (Fig. 6) are similar in form to conventional S - N curves, and (2) the crack initiation life increases along with the increases of tensile yield and ultimate stresses at cryogenic temperatures. The power laws of Eq. (1) and Eq. (2) for crack initiation and crack growth are also comparable, except that: (1) the exponents in the two equations have opposite signs, and (2) the coefficient in Eq. (1) is temperature dependent, whereas the coefficient in Eq. (2) is not.

Since our 6.2 mm thick specimens are not subject to linear elastic fracture at 4 K, we calculated residual strength values for the L-S orientation

266

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

4.4.2. Unidirectional crack growth


Fatigue crack growth rates for the superalloy were obtained for a wide range of AK, but we find the strongest temperature effects in the nearthreshold region. Lowering the temperature from 76 to 4 K raises AKTh by 4 MPa x ~/m (Fig. 7 Fig. 8 Fig. 9). In contrast, annealed austenitic stainless steels show little or no change in AK-rh for the same temperature reduction [8]. Theoretically, the cracking rate threshold does increase at cryogenic temperatures [20]. The reasons for a more pronounced effect in the superalloy are not perfectly clear, but two likely contributing factors are the exceptionally high yield strength of the superalloy at 4 K [8] and the metastability of the austenitic phase in stainless steels [11]. As stated earlier, the threshold improvement at cryogenic temperatures relates to kinks in the da/dN curve which mark the transition between the midrange and threshold regimes of crack growth. The effect is especially pronounced in the superalloy at 4 K. Various physical mechanisms have been advanced to explain similar behavior in other alloys. For example, one might expect the cracking rate dependence to change when, with decreasing stress intensity factor range, the cracktip plastic zone reaches a scale approaching the average grain size of the material. Further clarification of the behavior of the superalloy requires additional research beyond the scope of the present study.

4.4.3. Two-dimensional crack growth


Few data describing the flaw tolerance of conduits in the through-thickness direction have been published before [6]. Our study mainly features precracking in tension, which is representative of the type of loading currently foreseen in service applications. Based on the limited observations available to date, the propagation of surface cracks in this superalloy appears to follow closely the patterns documented by Corn [13] for selected steel, aluminum, and titanium alloys. During axial fatigue, cracks in the superalloy base metal quickly adopt and retain a nearly semicircular shape with aspect ratios near 0.9. The crack depth cannot be visually observed during an SCT test, but it can be inferred from measure-

ments of 2c, assuming a = 2c, based on the correlation shown in Fig. 11. The aspect ratio has little or no dependence on the increment Aa of growth. This approximation can be used in future magnet designs, as we shall illustrate in a second paper. From this work, the growth rate of fatigue cracks in extruded and heat-treated conduit is practically isotropic for the thickness and transverse directions. The use of fatigue data obtained from tests of conventional compact specimens is therefore justified for base metals. The behavior of superalloy welds has not yet been verified and warrants further study. Although the relationship a = 2c appears to be reliable for base metal specimens, it cannot be applied with equal confidence to superalloy welds. In two tests (unreported) the a/c ratios for axial fatigue cracks in weld specimens of our Ni-Fe superalloy were measured at 1.07-1.15, which is higher than base-metal values near 0.9. Since the tests used identical procedures and specimen geometries, the larger aspect ratios for welds might be attributable to microstructural factors or residual stresses. In this study, fatigue in 3-point bending produced precracks with a/c > 0.58. Bending fatigue permits the use of wider specimens and avoids cracking at the loading-pin holes or fillets. However, in bending, crack growth in the depth direction inflates the aspect ratio before cracking occurs on the surface or 2c direction. It is difficult or impossible to achieve lower aspect ratios (a/ c < 0.3) by this approach since the crack depth increases rapidly relative to crack length.

5. Conclusions

A new Ni-Fe superalloy was used to manufacture a seamless extruded conduit. This conduit has attractive cryogenic properties equivalent to those reported earlier for wrought developmental plates. The material behaves like other precipitation-hardened superalloys in that its mechanical properties are mildly temperature dependent and cryogenic effects are favourable. The strengthtoughness combination at 4 K is excellent (YS = 1155 MPa, JQ = 205 kJ m-2), and the threshold for fatigue crack growth is relatively high (10

R.L. Tobler et al./Fusion Engineering and Design 36 (1997) 251-267

267

M P a x x / m ) . S u r f a c e - c r a c k e d t e n s i o n tests using specimens o f full thickness (B = 6.2 m m ) d e m o n strate a d u c t i l e - f r a c t u r e m e c h a n i s m a n d g o o d c r a c k t o l e r a n c e in the t h r o u g h - w a l l direction. In fatigue, the resistance to the g r o w t h o f c r a c k s in the t h r o u g h - t h i c k n e s s d i r e c t i o n is n e a r l y equivalent to resistance in the t r a n s v e r s e direction, a n d this p r o m p t s the f o r m a t i o n o f semicircularly s h a p e d surface c r a c k s d u r i n g cyclic l o a d i n g in axial tension. T h e e m p i r i c a l o b s e r v a t i o n s i m p a c t fusion m a g n e t designs f a v o u r a b l y , as s h o w n in a s u b s e q u e n t p a p e r ( P a r t 2 o f this study). Thus, the new c o n d u i t a p p e a r s to be a n a t t r a c t i v e c a n d i d a t e for s u p e r c o n d u c t o r s h e a t h in fusion m a g n e t s . I m p l e m e n t a t i o n o f the m a t e r i a l will u l t i m a t e l y dep e n d o n its w e l d a b i l i t y a n d resistance to stressassisted grain b o u n d a r y o x i d a t i o n ( S A G B O ) ; b o t h o f these topics are c u r r e n t l y being r e s e a r c h e d a n d are b e y o n d the scope o f the p r e s e n t study.

Acknowledgements
T h e test m a t e r i a l a n d h e a t - t r e a t e d specimens were p r o v i d e d b y M I T with assistance f r o m L. T o m a . M e c h a n i c a l tests were p e r f o r m e d at N I S T with f u n d i n g f r o m the U S D e p a r t m e n t o f Energy, Office o f F u s i o n Energy.

References
[1] M.M. Morra, M.S. Thesis, Department of Materials Science and Engineering, MIT (1992). [2] M.M. Morra, R.G. Ballinger and I.S. Hwang, Incoloy 908, A low coefficient of expansion alloy for high strength cryogenic applications: Part I--Physical Metallurgy, Met. Trans., 21A(12) (1992) 3177-3192. [3] I.S. Hwang, R.G. Ballinger, M.M. Morra and M.M. Steeves, Mechanical properties of Incoloy 908--an update, Adv. Cryog. Eng. Maters., 38 (1992) 1-10. [4] N. Mitchell, Fatigue assessment of the structural steel in superconducting coils for Tokamaks, Fusion. Eng. Des., 19 (1992) 225-233. [5] L.S. Toma, I.S. Hwang, M.M. Steeves and R.N. Randall, Thermomechanical Process Effects on Hardness and Grain Size in lncoloy Alloy 908, Adv. Cryog. Eng. Maters., 40 (1994) 1307-1314.

[6] A. Nyilas, J. Zhang, B. Obst and A. Ulbricht, Fatigue and fatigue crack growth properties of 316 LN and Incoloy 908 below 10 K, Adv. Cryog. Eng. Maters., 38 (1992) 133-140. [7] A. Bussiba, R.L. Tobler and J.R. Berger, Superconductor conduits: fatigue crack growth rate and near-threshold behavior of three alloys, Adv. Cryog. Eng. Maters., 38 (1992) 167-174. [8] R.L. Tobler and I.S. Hwang, Fatigue crack thresholds of a nickel-iron alloy for superconductor sheaths at 4 K, Adv. Cryog. Eng. Maters., 40 (1994) 1315-1322. [9] A.R. Jack and A.T. Price, The initiation of fatigue cracks from notches in mild steel plates, Int. J. Fract. Mechs., 6 (1970) 401-409. [10] M. Creager and P.C. Paris, Elastic field equations for blunt cracks with reference to stress corrosion cracking, Int. J. Fract. Mechs., 3 (1968) 247-252. [11] R.L. Tobler, J.R. Berger and A. Bussiba, Long-crack fatigue thresholds and short crack simulation at liquid helium temperature, Adv. Cryog. Eng. Maters., 38 (1992) 159-166. [12] K. Suzuki, J. Fukakura and H. Kashiwaya, Nearthreshold fatigue crack growth of austenitic stainless steels at liquid helium temperature, Adv. Cryog. Eng. Maters., 38, (1992) 159-162. [13] D.L. Corn, A study of cracking techniques for obtaining partial thickness cracks of pre-selected depths and shapes, Eng. Fract. Mechs., 3 (1971) 45-52. [14] J.C. Newman and I.S. Raju, An empirical stress intensity factor equation for the surface crack, Eng. Fract. Mechs., 15 (1981) 185-192. [15] R.L. Tobler, Low temperature effects on the fracture behavior of a nickel base superalloy, Cryogenics, 16 (1974) 669-674. [16] W.A. Logsdon, J.M. Wells and R. Kossowsky, Fracture mechanics properties of austenitic stainless steels for advanced cryogenic applications, in: Proc. 2nd Int. Conf. Mechanical Behavior of Materials, ASM, 1976, pp. 12831289. [17] W.A. Logsdon, Cryogenic fracture mechanics properties of several manufacturing process/heat treatment combinations of Inconel x 750, Adv. Cryog. Eng., 22 (1977) 4758. [18] W.A. Logsdon, J.M. Wells and R. Kossowsky, The influence of processing and heat treatment on the cryogenic fracture mechanics properties of Inconel 718, Adv. Cryog. Eng., 24 (1978) 197-209. [19] W.A. Logsdon, J.M. Wells and R. Kossowsky, Cryogenic fracture toughness and fatigue crack-growth rate properties of Inconel 706 base material and gas tungsten-arc weldments, Adv. Cryog. Eng., 26 (1980) 137-150. [20] P.K. Liaw and W.A. Logsdon, Fatigue crack growth threshold at cryogenic temperatures: a review, Eng. Fract. Mechs., 22 (1985) 585-594.