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WELDING RESEARCH
D. K. HODGSON, T. DAI, and J. C. LIPPOLD are with The Ohio State University, Columbus, Ohio.
WELDING RESEARCH
Cladding
Autogenous Spot
WELDING RESEARCH
Std.
Elem. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Min. Max. Mean Dev.
C 0.133 0.108 0.115 0.131 0.153 0.153 0.153 0.145 0.157 0.119 0.156 0.121 0.168 0.111 0.147 0.143 0.108 0.168 0.138 0.019
Cr 2.34 2.15 2.39 2.26 2.54 2.35 2.36 2.39 2.18 2.16 2.2 2.11 2.17 2.33 2.39 2.47 2.11 2.54 2.23 0.127
Mo 1.02 0.94 1.08 0.9 1.19 1.03 1.03 0.97 0.95 0.97 0.94 0.99 0.96 0.88 1.06 1.05 0.88 1.19 1.00 0.077
Mn 0.49 0.445 0.435 0.347 0.533 0.537 0.542 0.563 0.73 0.416 0.473 0.485 0.758 0.429 0.519 0.544 0.347 0.758 0.515 0.106
Si 0.34 0.2 0.292 0.228 0.203 0.29 0.29 0.239 0.135 0.158 0.227 0.24 0.188 0.441 0.281 0.308 0.135 0.441 0.253 0.075
Ni 0.134 0.025 0.123 0.15 0.28 0.08 0.08 0.148 0.24 0.19 0.08 0.033 0.302 0.22 0.208 0.171 0.025 0.302 0.154 0.083
Cu 0.159 0.02 0.234 0.124 0.19 0.089 0.091 0.097 0.187 0.204 0.146 0.03 0.194 0.145 0.071 0.087 0.02 0.234 0.129 0.063
Sn 0.009 0.002 0.012 0.008 0.012 0.007 0.008 0.008 0.009 0.018 0.01 0.003 0.009 0.012 0.008 0.009 0.002 0.018 0.009 0.004
Al 0.027 0.021 0.025 0.025 0.023 0.024 0.023 0.022 0.02 0.002 0.016 0.027 0.022 0.004 0.022 0.021 0.002 0.027 0.02 0.007
V 0.018 0.016 0.016 0.018 0.021 0.016 0.017 0.02 0.016 0.014 0.016 0.014 0.017 0.016 0.018 0.017 0.014 0.021 0.017 0.002
Nb 0.004 0.003 0.004 0.006 0.021 0.003 0.004 0.003 0.004 0.004 0.004 0.003 0.003 0.004 0.004 0.004 0.003 0.021 0.005 0.004
Zr 0.002 0.002 0.002 0.001 0.002 0.002 0.002 0.002 0.002 0.002 0.002 0.001 0.002 0.002 0.002 0.002 0.001 0.002 0.002 0.000
Ti 0.003 0.002 0.003 0.002 0.002 0.003 0.003 0.002 0.001 0.002 0.002 0.002 0.002 0.003 0.002 0.002 0.001 0.003 0.002 0.001
B 0.0002 0.0001 0.0002 0.0001 0.0001 0.0002 0.0002 0.0002 0.0003 0.0001 0.0002 0.0001 0.0004 0.0001 0.0001 0.0001 0.0001 0.0004 0.0002 0.0001
P 0.013 0.01 0.011 0.013 0.009 0.007 0.008 0.011 0.008 0.009 0.009 0.012 0.007 0.014 0.014 0.009 0.007 0.014 0.01 0.002
S 0.01 0.017 0.017 0.003 0.004 0.003 0.004 0.003 0.008 0.02 0.018 0.021 0.009 0.012 0.01 0.009 0.003 0.021 0.0105 0.006
Ca 0.0005 0.0002 0.0004 0.0003 0.0008 0.0003 0.0003 0.0001 0.006 0.0002 0.0007 0.0002 0.0059 0.0005 0.0003 0.002 0.0001 0.006 0.001 0.002
Co 0.011 0.004 0.013 0.015 0.025 0.01 0.01 0.011 0.014 0.016 0.01 0.004 0.019 0.015 0.014 0.015 0.004 0.025 0.013 0.005
IIWCE 0.909 0.807 0.909 0.842 1.023 0.933 0.937 0.932 0.937 0.843 0.882 0.829 0.957 0.853 0.945 0.958 0.807 1.023 0.906 0.058
Pcm 0.366 0.311 0.354 0.34 0.41 0.384 0.385 0.376 0.387 0.333 0.371 0.329 0.403 0.336 0.381 0.383 0.311 0.41 0.366 0.029
Table 2 — Parameters for Autogenous GTAW Spot Weld kg Vickers microhardness indents
(VHN1.0). For each tempering treatment
Preheat Temperature Ambient of each heat, a microhardness traverse
from the fusion zone to the base mate-
Welding Current 100 A
Arc Length 2.54 mm rial was used to measure the hardness
Voltage (approx.) 11.5–12 V as a function of the distance from the
Hold Time 5s fusion boundary. Indents for these trav-
Shielding Gas 99.99% Ar erses were made with a 100-g load
(VHN0.1) and a spacing of 75 m. These
of 1350°C. The peak temperature was The furnace used was a horizontal Lind- values were also used to calculate an av-
maintained for 1 s or 10 s before allow- berg 59544 type. At the end of the tem- erage hardness of the HAZ for each
ing the sample to free cool. The free pering time, samples were quenched in tempering treatment.
cooling resulted in a Dt8–5 in the range room temperature water. (Equation 3 is Optical microscopy. After hard-
from 7.5 to 9.5 s and was controlled by the Holloman-Jaffe parameter (HJP) ness testing, samples were mounted in
the free span between the two copper for tempering treatments). Bakelite and ground using successive
jaws of the Gleeble. steps of 320-, 400-, and 600-grit wet
Tempering heat treatment. To HJP = T * (20 + LOG(t)) (3) silicon carbide abrasive papers and
determine the response of each heat to polished with 9-, 6-, 3-, and 1-m dia-
tempering heat treatments, samples Hardness testing. The as- mond polishing paste. After a suitable
were subjected to the seven tempering quenched hardness of each heat of ma- surface was obtained, samples were
heat treatments shown in Table 3. terial was measured on the Rockwell C chemically etched using Vilella’s etch
These heat treatments were selected to scale using a Leco LR series hardness (5 cc HCL + 2 g picric acid + 100 cc eth-
represent Hollomon-Jaffe tempering tester. Prior to indenting, the samples yl alcohol) or 2/5% nital (2–5% nitric
parameters that span a postweld heat were sectioned through the centerline acid + ethyl alcohol) to increase con-
treatment procedure common in indus- and another parallel plane in order to trast of microstructural features.
trial production (HT-3 in Table 3). ensure a flat, parallel surface for accu-
These values were calculated using rate measurements. An average hard- Results and Discussion
Equation 3 with temperature (T) in ness was calculated based on four in-
kelvin and time (t) in hours (Ref. 4). dents near the center of the cross sec- Hardness of as-quenched and
During procedure development, ther- tion. Because of the smaller area, the simulated heats. The three separate
mocouple monitoring determined that simulated CGHAZ samples were meas- solution austenization treatments were
samples reached furnace temperature in ured with 100-g-load Vickers micro- evaluated for each heat by comparing
approximately 20 min. This heating hardness. Due to low hardness that pre- the hardness of the as-quenched mi-
time was not considered in the calcula- vented the use of the Rockwell C scale, crostructure. Because F22 transforms to
tion of the Hollomon-Jaffe parameters. the base material was measured with 1- mostly martensite during high cooling
WELDING RESEARCH
WELDING RESEARCH
WELDING RESEARCH
peak temperature farther from the fu- stages of tempering (Ref. 8). It
sion boundary in the fine-grained HAZ is of note that despite similar
(FGHAZ) results in less precipitate dis- carbon content and carbon
solution and therefore a lower level of equivalent, Heat 5 (0.153 wt- Fig. 8 — Heat 5 (0.153 wt-% C - top) and Heat 7
carbon to contribute to transforma- % C) and Heat 7 (0.153 wt-% (0.153 wt-% C - bottom) hardness traverses in the as-
tion strengthening by the formation C) have different hardness dis- welded and tempered condition.
of martensite (Ref. 9). tribution within the HAZ with
The dissolution of the precipitates Heat 5 (0.153 wt-% C) being signifi- until the hardness measurements
in the CGHAZ also allows for more cantly harder in the coarse-grained re- converged during HT-5 and HT-7.
grain growth within the CGHAZ. The gion through all of the tempering treat- While the general trend for the
resulting larger grain size in the ments. tempering treatment is lower hardness
coarse-grained region increases the Further tempering resulted in ad- with a higher Hollomon-Jaffe parame-
hardenability of the region as well as ditional softening of the microstruc- ter, there are some heat treatments
reduces the contribution to strength- ture. Figure 9 shows the reduction of that result in a secondary hardening
ening from a Hall-Petch effect due to the average hardness of a selection of effect. This phenomenon is particular-
the larger martensite block size (Refs. the autogenous spot welds and simu- ly evident in the difference in hardness
10–13). The hardness of the fusion lated CGHAZs. The spot welds shown in the spot weld samples between HT-
zone region of the autogenous spot consist of those with the lowest car- 3 and HT-4, despite both heat treat-
welds was also measured and exhibited bon content (Heat 2 – 0.108 wt-% C), ments being conducted at the same
the highest hardness of any of the highest carbon content (Heat 13 – temperature of 638°C. Secondary
samples tested. Since this region was 0.168 wt-%), lowest as-tempered hardening has been observed in
completely melted, any precipitates hardness (Heat 10 – 0.119 wt-% C), molybdenum containing low-alloy
(carbides) would fully dissolve. This highest tempered hardness (Heat 5 – steels and has been attributed to the
would result in the highest possible 0.153 wt-% C) and two additional formation of Mo2C carbides (Ref. 14).
amount of carbon free to contribute to heats of nearly identical composition This particular molybdenum-rich car-
transformation strengthening. (Heats 6 and 7 – 0.153 wt-% C). As bide can result in an increase in hard-
Hardness of tempered heats. The expected, the general trend is for the ness due to the matrix coherency in
tempering treatments selected were ef- hardness to decrease as the Hol- the early stages of precipitation. Baker
fective in reducing the hardness of all lomon-Jaffe parameter is increased. and Nutting’s investigation into the
regions of the autogenous weld samples The simulated CGHAZ samples re- tempering sequence in 2.25Cr-1Mo
as shown in Fig. 8 for Heats 5 (0.153 sulted in approximately the same av- steel confirms that in the time and
wt-% C) and 7 (0.153 wt-% C). As can erage tempering rate as the spot temperature range of both HT-3 and
be seen, significant reduction in hard- welds of the same heat for three of HT-4, Mo2C-type carbides are present
ness occurs even at the lowest temper- the four heats tested. Heat 5 (0.153 in quenched and tempered martensitic
ing temperature and time (638°C/1 h), wt-% C) had a higher tempered hard- microstructures (Ref. 15) — Fig. 10.
which is consistent with Speich who ness at each Holloman-Jaffe parame- Even when tempering at the high-
found that the drastic reduction in ter until the values converged during est Hollomon-Jaffe parameter, the as-
hardness results from the decomposi- the most severe treatment while Heat tempered hardness often did not meet
tion of the martensite by the formation 10 (0.119 wt-% C) was noticeably the 22 HRc or 250 VHN hardness re-
of M3C carbides during the initial softer earlier in the tempering cycle quirement set forth by NACE
WELDING RESEARCH
Fig. 9 — Average heat-affected zone and simulated coarse-grain Fig. 10 — Precipitation sequence of F22 in the quenched and
heat-affected zone tempering response. tempered condition (Ref. 15). (The Journal of the Iron and Steel
Institute).
MR0175. Several factors contribute to was effective in dissolving base metal Uhlig’s Corrosion Handbook. Wiley.
the actual industrial postweld heat precipitates and achieving predicted 3. Lippold, J. C., and Fusner, E. 2010.
treatment being more effective than as-quenched hardness levels. Unpublished research. Columbus, Ohio:
the experiments conducted here. In The average as-welded hardness of The Ohio State University.
4. Hollomon, J., and Jaffe, L. 1945.
most cases, the corrosion-resistant the HAZ and fusion zone exceeded
Time-temperature relations in tempering
cladding is deposited in two passes, that of the austenitized and quenched steel. Metal Technology 12: 223–249.
which would result in a high-tempera- base materials. 5. Krauss, G. 1999. Martensite in steel:
ture tempering effect of the second Most of the heats evaluated in this Strength and structure. Materials Science
pass on the HAZ of the first pass. Ad- study did not reach 250 VHN during and Engineering A 273–275: 40–57.
ditionally, since the target compo- tempering at 638° and 677°C (1180° 6. Jaffe, L., and Gordon E. 1957. Tem-
nents are typically large, the heating and 1250°F) for times up to 11 h. perability of Steels, Transactions. American
and cooling rates of the actual parts A secondary hardening reaction re- Society for Metals 49: 359–371.
are much slower than those of the sulting from precipitation of Mo2C op- 7. Bhadeshia, H. 1983. Carbon content
small laboratory samples. This will in poses the tempering effect predicted of retained austenite in quenched steels.
Metal Science 17: 151–152.
effect increase the Hollomon-Jaffe pa- by the Holloman-Jaffe parameter.
8. Speich, G. 1969. Tempering of low-
rameter, even for the same soak time carbon martensite. Trans Met Soc AIME
heat treatment. Since HT-3 is based on
Acknowledgments 245: 2553–2564.
a postweld heat treatment cycle com- 9. Cottrell, A., and Bilby, B. 1962. Dislo-
monly used in industrial practice, the cation theory of yielding and strain ageing
secondary hardening effect could be a This work was supported by of iron. Proc. Phys. Soc. A 62: 49–62.
contributor to difficulty in meeting Cameron International (now OneSub- 10. Doane, D. 1979. Application of hard-
the maximum hardness requirement sea) through the NSF I/UCRC for Inte- enability concepts in heat treatment of steel.
by resulting in an unexpected increase grated Materials Joining Science for Journal of Heat Treating 1(1): 5–30.
in hardness near the end of the tem- Energy Applications (CIMJSEA). Spe- 11. Sylwestrowicz, W., and Hall, E.
1951. The deformation and ageing of mild
pering treatment. cial thanks to Mr. Dean Hannam from
steel. Proc. Phys. Soc. B 64(6): 495–502.
OneSubsea who arranged for the pro- 12. Petch, N. 1953. The cleavage
curement of the F22 materials and
Conclusions provided valuable insight and support
strength of crystals. Journal of the Iron and
Steel Institue 173: 25–28.
throughout the course of the study. 13. Morito, S., Yoshida, H., Maki, T.,
Solution austenization treatments of and Huang, X. 2006. Effect of block size on
954°C for 1 h, and 1148°C for 1 and 4 h References the strength of lath martensite in low car-
were not sufficient to promote total dis- bon steels. Materials Science and Engineer-
solution of preexisting precipitates in all ing A 438-440: 237–240.
base material heats and achieve the ex- 14. Speich, G. R., and Leslie, W. C.
1. Berkowitz, B., and Heubaum, F. 1984. 1972. Tempering of steel. Metallurgical
pected as-quenched hardness. This ef- The role of hydrogen in sulfide stress Transactions 3(5): 1043–1054.
fect was most pronounced at carbon cracking of low alloy steels. Corrosion 15. Baker, R., and Nutting, J. 1959. The
levels above 0.14 wt-%. 40(5): 240–245. tempering of 2.25Cr-1Mo steel after
A simulated weld thermal cycle 2. Elboujdaini, M. 2000. Hydrogen-in- quenching and normalizing. The Journal of
with a peak temperature of 1350°C duced cracking and sulfide stress cracking. the Iron and Steel Institute 192: 257–268.