austenitic

stainless steels
during long-term
aging

The microstructural changes, precipitation behaviour, and mechanical properties

of typical austenitic stainless steels (304 H, 316 H, 321 H, 347 H, and
Tempaloy A-1) have been examined after long-term aging. The steels were aged
statically in the temperature range 600-800C for up to 50000 h. The
microstructural changes were observed by optical and transmission electron
microscopy, and the extracted residue was identified using X-ray analysis.
Time-temperature precipitation diagrams were made for each steel. The amount
of (j-phase was measuredinsamples aged at 700C. The hardness and impactvalue changes, and the tensile properties of aged samples were measured.
MSTj358

Y. Minami
H. Kimura
Y. Ihara

1986 The Institute of Metals. Manuscript received 9 September 1985. The

authors are in the Technical Research Centre, Nippon Kokan K.K., Kawasaki,
Japan.

M icrostructu ral

changes in

Introduction

Experimental

Austenitic 18Cr-8Ni stainless steels have better strength

and oxidation resistance at high temperatures than lowalloy and carbon steels, and are less expensive than
Ni-base alloys. For this reason they have been used for
high-temperature components, such as superheater and
reheater tubings of conventional fossil fuel fired boilers,
reformer tubings of chemical and petrochemical plants, and
high-temperature parts of nuclear reactors. They have a
service life of several (sometimes over ten) years.
For such applications, strength at high temperature,
especially long-term creep rupture strength, is the most
important property, and determines the life of the
components. The evaluation of degradation and remaining
life is required for maintenance purposes, and for this the
service conditions, i.e. applied stress, time, and
temperature, must be known. The exposed temperature of
the materials is particularly difficult to determine since the
temperature is not constant during the service period in
most practical operations.
Materials undergo mechanical, physical, and metallurgical changes when exposed to certain service
conditions, and by examining these changes inversely, it is
possible to evaluate the actual service conditions,
degradation, and remaining life of the material. However,
very few of the reference data required for this kind
of evaluation exist, especially from samples aged
systematically for the length of the actual service period.
The present study examines the metallurgical and mechanical changes in the typical 300 series of austenitic stainless
steels and in 18Cr-l0Ni-Ti-Nb (Tempaloy A-l*), which
has higher long-term creep rupture strength than the other
steels, 1 and their long-term precipitation behaviour has
also been clarified.

MATERIALS
Several austenitic stainless steels (304 H, 316 H, 321 H,
347 H, and Tempaloy A-I, chemical compositions given in
Table 1) were melted in a 40 t electric furnace and rolled
into billets for tubings. A part of each billet was sliced and
hot-rolled into 15 mm thick plate for laboratory testing.
The base composition of Tempaloy A-I is similar to that
of steel 304 H, with small additions of Ti and Nb. Solution
treatments were conducted, followed by water cooling. In
order to examine the long-term precipitation behaviour,
the samples were aged at 600-800C for up to 50000 h.

* Tempaloy A-I, a modification of steel 304 H, is a registered trademark of

Nippon Kokan K.K.
Table 1

Chemical compositions,

X-RAY DIFFRACTION
A solution of 10% acetyl acetone was used to extract the
precipitated residues of the aged samples. X-ray diffraction
analysis was carried out using a Philips diffractometer.
CALCULATION OF u-PHASE
After optical observation, the samples were repolished and
etched using a 10% KOH solution so that only the (j-phase
would be coloured. The amount of (j-phase was then
measured using an automatic area calculator (Quantimet).
MECHANICAL PROPERTIES
Tensile and 2 mm V-notch Charpy specimens were
prepared from the aged plates. Tensile testing was
performed at room temperature and Charpy testing at OC.
Vickers hardness was measured with a 50 kg load at five
points on each sample.

wt%, and solution treatments

Materials

Si

Mn

Cr

304 H
316 H
321 H
347 H
Tempaloy

005
005
005
005
007

060
063
059
059
066

173
181
176
164
171

0028
0029
0024
0019
0028

0012
0010
0008
0014
0005

187
166
176
176
180

A-1

METALLOGRAPHIC OBSERVATION
Cubic samples 15 x 20 x 20 mm taken from the aged plates
were mechanically polished, etched in 10% oxalic acid, and
observed by optical microscopy. Thin foils, prepared using
the twin jet method with perchloric acid were examined
using transmission electron microscopy (TEM).

Mo

23

of steels studied
Ni

90
119
105
104
98

0026
0024
0011
0025
0033

Nb

087
013

Ti

Solution

035

1050C
1100C
1100C
1100C
1100C

006

treatment
for
for
for
for
for

30
30
30
30
30

min,
min,
min,
min,
min,

WO
WO
WO
WO
WO

WO water quenched.

Materials Science and Technology

August 1986

Vol. 2 795

796

Minami et al.

Long-term aging of austenitic stainless steels

,,'

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Materials Science and Technology

August 1986

Vol. 2

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Minami et al.

Long-term

aging of austenitic

stainless steels

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Materials Science and Technology

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August 1986

'+i
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Vol. 2

798

Minami et al.

Table 2

Long-term

aging of austenitic

X-ray
diffraction
results
for
annealed for 10000 h at 750C

Observed
d
268
263
239
227
218

M
M
M
W
M

212

205
201
197
193
189
186
180

S
W
W
W
M
W
M

177

169
163
161

W
W
W

Table 3

304 H

steel

Cr23C6 (ASTM 14-407)

a-phase

(ASTM 5-708)

hkl

226

002

hkl

266

400

30

237

420

50

217

422

50

205

511

100

188

440

50

180
178

531
600
442

40

163
161

533
622

5
30

206
202
196
193
188

80
60
80
100
80

176

312

10

304 H steel
The optical microstructure of the aged samples of 304 H
steel is shown in Fig. 1. For lower aging temperature
and/or shorter aging time, precipitates were observed only
at grain boundaries. The fine precipitates near grain
boundaries increased with higher temperature and longer
time. Some (J - particles were observed using optical
microscopy on the samples aged for 50000 h. These were
formed mostly at the triple points of grain boundaries and
their average size was '" 10 ~m. The TTP diagram for
304 H steel is also shown in Fig. 1. The only precipitate
found after aging for a short period was M23C6, but after

100

results for 316 H steel annealed for 10000 h at 750C

14-407)

hkl

237

420

Fe2Mo (ASTM 6-622)

237
230
222
218

M
W
W
S

214

209
205
202
198
194
189
181

S
S
S
S
W
S
M

178

178

174
169
161

W
W
W

163
161

. Omitted

because of their low 1/10 ratio (= 1).

217

OPTICAL MICROSTRUCTURE AND

X-RAY ANALYSIS
The X-ray diffraction results are given in Tables 2-6, and
time-temperature
precipitation (TTP) diagrams were
drawn using the identified phases.

50

Cr23C6 (ASTM

Observed

Results and discussion

10

112
410
330
202
212
411
331

213

X-ray diffraction

Table 4

stainless steels

50

422

50

hkl

236

110

218

x-FeCrMo

60

103

(ASTM

6-676)

a-phase

h2+k2+

,2

hkl

237

14

20
2'26

002

10

222

16

10
213

112
410

100

330
202
212
411
331
222

80
60
80
100
80
10

312

10

100

209
205

511

188
180

100

440
531
600
442

TiC
(ASTM

hkl

004
100
102

2'49
2-47
237
229
223
216

S
M
W
M
S
S

2'49

213

205
203
198
193
188
187
180

M
M
M
M
W
M
W

TiN
(ASTM

6-614)
hkl

103

10

251

111

22
24

50
30

174

26

40

176

6-642)
hkl

Cr23C6
(ASTM

14-407)

a-phase
(ASTM 5-708)

hkl

hkl

266

400

30

237

420

50
226

002

80

200

111

77

100

217
212

187

189
181

104

006

50

200

. Omitted

M
M

161
154

110
106

60
20

220

50

because of their low 1/10 ratio (= 1).

Materials Science and Technology

August

1986

Vol. 2

50
213

205

511

100

188

440

50

180

531
600
442
533
622

163
161
154

422

100

178

161
157

10

100
218

198

40

50

2-44

223

20

results for 321 H steel annealed for 5000 h at 700C

16-849)

278

199

206
202
196
193
188
183

5
30

Ti4C2S2
(ASTM

60
100
60

100

18

40

Observed

278

200
112
201

50
50

533
622

X-ray diffraction

205
202
198

(ASTM 5-708)

206
202
196
193
188

'

112
410
330
202
212
411
331

80
60
80
100
80

312

10

100

50
40
5
30

176

Minami et al.

Long-term aging of austenitic stainless steels

799

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800

Minami et a/.

Table 5

Long-term

X-ray diffraction

10-181 )

NbC (ASTM

hkl

258

111

W
S
W
M
S
S

214

209
2.06
204
200
198
194
189
185
178

W
M
W
W
M
M
M
W
W

158
147

S
W

Omitted

223

158

stainless steels

results for 347 H steel annealed for 25000 h at 700C

Observed

261
258
242
231
223
218

aging of austenitic

200

220

17-908)

Fe2Nb (ASTM

FeaNbaC (ASTM

hkl

2'41

110

50

222

103

70

17-128)

hkl

261

331

230

442

80

217

511

100

80

208
205

200
112

10
100

201
196

201
004

60
10

50

hkl

226

002

10

213

112
410

100

206
202

330
202

80
60

196
193
188
183
176

212
411
331
222
312

80
100
80
10
10

50

200

440

80

188

442

50

179
170
158
147

620
622
551
731

10
50
80
80

because of their low 1/10 ratio (= 1).

316 H steel
The optical microstructure of 316 H steel is shown in
Fig. 2. The trend of the microstructural change was similar
to that of 304 H steel, although the precipitates in the
matrix were more abundant. A precipitate-free zone
formed near a-particles, as can be seen after aging for
50000 h at 700C.
The TTP diagram for 316 H steel is also given in Fig. 2.
Its precipitation behaviour is more complex than that of
X-ray diffraction

Table 6

results for Tempaloy

TiN (ASTM 6-642)

NbC (ASTM

hkl

258

111

267
256
245
239
227
222
216

W
M
M
S
W
M
S

213

244

hkl

111

304 H because of the Mo-bearing precipitates such as

Fe2Mo (Laves phase) and Fe1SCr6Mos (x-phase). At lower
aging temperature the precipitation of Fe2Mo occurred
before the precipitation of a-phase. The precipitation of
x-phase was detected at above 700C. The x- and
a-precipitates remained at 800C, while Fe2Mo disappeared, as can be seen from the C-curve characteristic.
Particles of a-phase (the dark area in the optical microstructure) formed at triple points of grain boundaries in the
same way as in 304 H steel, although they were slightly
smaller in size.
The precipitation behaviour of 316 H steel for shorter
aging time has been studied by Weiss and Stickler, 3 and
their observations show good agreement with the results
of the present study. Lai4 has also studied the precipitates
in cast 316 H and has obtained similar results for Fe2Mo
phase dissolving over 800C. The u-phase precipitation was
not reported by Lai to occur above 700C, although it was
detected at 800C in the present study.

A-1 steel annealed for 25000 h at 750C

Observed

10-181)

Cr23C6 (ASTM
d

hkl

266

400

30

237

420

50

200

422

511

100

197
193
188
183
180

W
W
M
W
M

188

440

50

180

178

178

531
600
442

40

175
163
161
156

W
W
M
W

163
161

533
622

5
30

150

149

551
711

158

220

56

because of their low 1/10 ratio (= 1 ).

Materials Science and Technology

002

10

213

100

206
202
196
193
188
183

112
410
330
202
212
411
331
222

176

312

10

50

100
205

220

226
80

150

hkl

100

217
200

77
223

212

O"-phase (ASTM 5-708)

14-407)

205

Omitted

100

aging for over 1000 h, M23C6 and a-phase were detected.

Biss and Sikka2 have studied creep ruptured specimens of
steel 304 H after aging for 49000 hand 59900 h at 595C,
and report the precipitation of M6C, M23C6, and a-phase
for 49000 h, and M23C6 and a-phase for 59900 h. They
suggest that M6C forms at grain boundaries and then
dissolves because of the growth of a-phase, but in the
present study, M6C was not detected for any aging
conditions.

O"-phase (ASTM 5-708)

August

1986

.Vol. 2

80
60
80
100
80
10

50

50

Long-term aging of austenitic stainless steels

Minami et aI,

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Materials Science and Technology

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Vol. 2

802

Minami et al.

Long-term

aging of austenitic

stainless steels

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Minami

M23C6 in matrix
at 750C

of 316 H steel annealed

for 50000 h

321 H steel
The optical microstructures

and TTP diagram

of aged

samples of 321 H steel are shown in Fig. 3. For lower

temperature and/or shorter aging time, precipitates were
seen only at grain boundaries, as with 304 Hand 316 H.
No precipitate-free zone such as those observed near the
grain boundary in 304 Hand 316 H were identified in the
intermediate aging conditions. At higher temperature and
for longer aging time, massive a-particles were formed.
Although five types of precipitate were identified by
X-ray analysis, TiN and Ti4C2S2 were excluded from the
TTP diagram since they already existed in the solution
treatment condition. Although the value of Ti/C was larger
than the stoichiometric ratio, a small amount of M23C6
type carbide was detected. Precipitates of M23C6 were also
reported by Grot and SpruielP in 321 H with a larger value
for Ti/C than the stoichiometric ratio. TiC was found for
all aging conditions and a-precipitation occurred earlier
than with 304 Hand 316 H.
Lai6 found G-phase (fcc Ni- Ti-Si) in high-silicon finegrained steels, and reported that precipitation could be
inhibited by larger grain size. The G-phase was not
detected in the present study, possibly because the grain
size was sufficiently large and the silicon content
sufficiently low for it not to have formed.

et al.

Long-term

aging of austenitic

stainless steels

803

x-phase in 316 H annealed for 50000 h at 750C

observed, the grain size being smaller than that of 321 H,

so increasing the number of the triple points of grain
boundaries preferred for the precipitation of a-particles.
The precipitates in 347 H are summarized in the TTP
diagram. Using the conventional X-ray technique it is
difficult to distinguish the undissolved NbC at solution
temperature from the fine NbC formed during aging, and
hence both types are marked without distinction in the
figure, as for the TiC in 321 H. The precipitation of
a-phase started slightly earlier than in 321 H, and not
only at the triple points of grain boundaries but also
on the grain boundaries themselves. The intermetallic
compound Fe2Nb (Laves phase) was identified after
a-phase precipitation, and this was followed by the
precipitation of M6C type carbide. The Fe2Nb disappeared
after aging for longer periods at higher temperatures. The
precipitation conditions for Fe2 Nb are indicated by arrows
in Fig. 4.

347 H steel
The optical microstructure and TTP diagram of 347 H
steel is shown in Fig. 4. The microstructural change had a
similar tendency to that of 321 H. Many a-particles were

Tempaloy A-1
The optical microstructure and the TTP diagram of
Tempaloy A-1 are shown in Fig. 5. The microstructural
change is almost the same as that of 304 H. Precipitation of
M23C6 near grain boundaries is not observed. Both M23C6
and NbC carbides were detected at all aging conditions,
and a-phase particles were formed at the triple points of
grain boundaries after longer aging times at higher
ternpera tures.
Though a small amount of Ti was added to this steel,
TiC was not detected. It could be concluded that Ti was
compounded in a form such as (Ti, Nb )C, since Ti was

M23C6 on grain boundary

for 10000 h at 750C

of Tempaloy

A-1 annealed

a-phase and string-like

for 5000 h at 700C

TiC in 321 H steel annealed

804

Minami

et ale Long-term

aging of austenitic

stainless steels

M23C6 and MC in matrix

for 10000 h at 750C

of Tempaloy A-1 annealed

term aging. This tendency was also found in 304 Hand

Tempaloy A-I. At grain boundaries M23C6 type carbides
aggregated to form block-like shapes (Fig. 7).
The coarsened, rod~shaped x-phase precipitated in 316 H
aged at 750C for 50000 h is shown in Fig. 8. It is
considerably larger in size than the M23C6 precipitated
under the same conditions.
Blocky O"-particlesof '" 3 ~m dia. at the grain boundary
in 321 H aged at 700C for 5000 h are shown in Fig. 9,
where the string-like precipitates of TiC on dislocations
can also be seen.
The precipitates in 347 H aged at 700C for 10000 hare
shown in Fig. 10. Block-like precipitations of M6C are
found on the grain boundary (Fig. lOa), in the matrix
rod-like particles of Fe2Nb have formed (Fig. lOb), and
NbC is found in a chain-like formation after long-term
aging (Fig. 10c).
Figure 11 shows M23C6 and fine MC carbides in
Tempaloy A-1 aged at 750C for 10000 h. The MC
carbide in Tempaloy A-1 is considerably finer (",45 nm
average dia.) than the NbC in 347 H ('" 80 nm after aging
for 50000 h at 750C), and it is expected that the presence
of this fine MC carbide will contribute to the long-term
creep rupture strength of the material.

a
10

M6C on grain boundary; b Fe2Nb in matrix; c NbC in matrix

Precipitates
700C

in 347 H steels annealed for 10000 h at

found not to be included in NbC by energy dispersed X-ray

(EDX) analysis. The MC type carbide was identified as
NbC by lattice parameter measurement. F or this reason,
MC carbide was indicated as NbC in Fig. 5.
The microstructural change in Tempaloy A-1 seemed to
be smaller than that of the other steels. This microstructural stability is considered to be important for long
term creep rupture strength.
TRANSMISSION
ELECTRON MICROSCOPIC
OBSERVATION
Several typical precipitates of the aged samples are shown
in Figs. 6-11. Some M23C6 type carbide was found in the
matrix of 316 H aged at 750C for 50000 h (Fig. 6) which
precipitated in cubic shape, with an average size of about
02p,m. They coarsened and became chain-like after long-

Materials Science and Technology

August

1986

Vol. 2

PRECIPITATION OF (T-PARTICLES
The growth of precipitated O"-phaseat 700C is shown in
Fig. 12. Rapid. growth occurs over 1000 h in 321 Hand
347 H, while in 304 H, 316 H, and Tempaloy A-1 it is
retarded until 10000 h. The greatest amount of O"-phase
was observed in 347 H: about 5% at 50000 h.
Barcik 7 has suggested that O"-phaseprecipitation occurs

347
5
-321
A-1

316
304

103
104
AGING TIME AT 700C,h
12

Growth

of a-phase at 700C

Minami et al.

200

o 304H
~ 316H
321 H

180

Long-term

aging of austenitic

stainless steels

805

, 347H

o t(Zmpaloy

A-1

800
N

0> 160

IE

o
.!9

~600

.x.

140

>
I
uf

r~ 400

(a)

120
~200

~r-

fE

180

(f)

200

<!

160

0 ...

140

<!

w
~

120

<!

103
104
AGING TIME,h

unagoo
condition

a 650C
13

LL

o
Z
o

anneal; b 700C anneal

Hardness after aging at different

up to 50000 h

temperatures

6~

for

~
more slowly in coarse- than fine-grained steels, and 347 H
was indeed fine-grained in this study. The grain size of
Tempaloy A-1 was also fine, but the amount of a-phase
was almost equal to that of the other coarse-grained steels.
It was therefore concluded that the main factor determining the amount of precipitation was the phase stability,
i.e. the balance of ferrite/austenite forming elements.
MECHANICAL PROPERTIES
Hardness
The hardness of the specimens aged at 650 and 700C for
up to 50000 h is shown in Fig. 13. In all steels there was a
trend for hardness to increase with aging time, especially in
316 H.
The increase in hardness can be explained in general as
follows. For the shorter time, the main hardening factor is
the carbide, since no other precipitate was found. For the
longer time, hardening from carbides is slightly reduced
because of their coarsening, while a-precipitation occurs,
considerably contributing to the increase in hardness.
Hence, the hardness increases according to the aging time.
In 316 H, the precipitation of Fe2Mo and x-phase gives
rise to a further increase. Although Fe2Nb in 347 H may
also increase the hardness, its effect is not great because of
its smaller precipitated amount.
Toughness
Toughness decreased according to aging time in all
materials. Figure 14 shows the change in the toughness in
304 Hand 347 H, which exhibited the highest and the
lowest values, respectively. The decrease in toughness can
be explained in a similar way to the increase in the
hardness, and moreover, it is recognized that the formation
~E400

J_300
w

304H
347H

~200

rU 100

40

800

unagC2d

condition
AGING TEMPERATURE

15

FOR 10000

h,oC

Room temperature tensile properties of 304 Hand

316 H steels after aging for 10000 h at 60G-SOOoe

of a-phase led to the reduction in toughness. The existence

of Fe2Mo and x-phase in 316 H did not have as great an
effect on toughness as on hardness.
Tensi Ie properties
Figure 15 shows the tensile properties of 304 Hand 316 H
aged for 10000 h in the temperature range 600-800C.
Other steels showed properties intermediate between 304 H
and 316 H. The tensile and 02% proof strength did not
vary with aging temperature, while the reduction of area
decreased at higher temperature, particularly above 700C
in 316 H.

Conclusions
The metallographic and mechanical changes of typical
austenitic stainless steels aged at 600-800C for up to
50000 h have been studied, with particular attention being
paid to their precipitation behaviour.
1. The carbides which precipitated in the aged 304 H
and 316 H steels were M23C6 According to Mo addition
Fe2Mo and x-phase also precipitated in the 316 H steel.
2. MC carbides were the main precipitate in steels
containing additions of Ti or Nb, i.e. in 321 Hand 347 H
steels. In 347 H steel, Fe2Nb and M6C were also identified.
3. Both M23C6 and MC precipitated in Tempaloy A-1,
the precipitated size of MC being relatively smaller than
that in the 321"H or 347 H steels.
4. The precipitation of a-phase started earlier in the
321 Hand 347 H steels than in the other steels tested.
Aging at 700C, a-phase appeared after about 500 h in the
321 Hand 347 H steels, and after about 5000 h in the
304H, 316H, and Tempaloy A-1 steels. The precipitated a
was considered to be deleterious to toughness.

unagC2d

condition

14

103
104
AGING TIME, h

Impact value of 304 Hand

at 700 e
0

105

347 H steels after aging

References
1.

Y. MINAMI, H. KIMURA,

Syst., 1985, 7, (1), 45-54.

and

M. TANIMURA:

J. Mater. Energy

806

Minami et al.

Long-term

aging of austenitic

stainless steels

A. BISS and v. K. SIKKA: Me tall. Trans., 1981, 12A,

1360-1362.
3. B. WEISS and R. STICKLER: Me tall. Trans., 1972, 3, 851-866.
4. J. K. LAI: Mater. Sci. Eng., 1983, 58, 195-209.

2.

v.

5. A. S. GROT and J. E. SPRUIELL: Me tall. Trans., 1975,

2023-2030.
6. J. K. LAI: Mater. Sci. Technol., 1985, 1,97-100.
7. J. BARCIK: Me tall. Trans., 1983, 14A, 635-641.

Forthcoming Publication

Materials Science and Technology

August

1986

Vol. 2

6A,