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Journal of Materials Processing Technology 162163 (2005) 342349

The influence of niobium and aging treatment in the


18% Ni maraging steel
D.G. Lee a, , K.C. Jang a , J.M. Kuk a , I.S. Kim b
b

a Korea Institute of Industrial Technology, P.O. Box 1, Chumdan-dong, Gwangsan-gu, Gwangju 506-824, Korea
Mechanical Engineering Department, Mokpo National University, 61 Torim-ri, Chonggye-myon, Muan-gun, Chonnam, Korea

Abstract
Effects of Nb (niobium) contents and aging conditions on the strength and fatigue life of 18% Ni maraging steel commonly using in aircraft,
space field, nuclear energy, and vehicle, etc. were investigated. Hardness value decreased about 3% for annealed specimens and increased
about 60% for 1 h aged specimens. But the values of the other specimens aged 2 h or more showed almost the same. The yield strength was
the highest about 1800 MPa in 0.06% Nb specimen having twice as much as the base metal specimen. Also, the elongation was the highest
in 0.03% Nb specimen showing the same as base metal specimen. The higher aging temperature and the longer aging time, the fatigue life
increased. On the other hand, the 0.03% Nb specimen showed the highest fatigue life which increased about 12% more than base metal
specimen. 0.06% Nb specimen aged at 482 C for 8 h simultaneously satisfied the 250 grade strength and 200 grade elongation having the
most superior mechanical properties.
2005 Elsevier B.V. All rights reserved.
Keywords: GMAW; Niobium content; Solution annealing; Age hardening; Yield strength; Fatigue life

1. Introduction
Recently the needs of high reliable substances of high
strength and high ductility are gradually increased with the
development of aerospace industry [1]. The characteristics of
this grey and white steel has high ductility, formability, corrosion resistant and high temperature strength, and is easy to
fabricate, weld and treat with heat, and maintain an invariable
size even after heat treatment [2,3].
Maraging steels having 18% Ni are divided into two broad
classes depending on the primary strengthening element in
the chemical analysis. The original maraging steels, introduced in the early 1960s, depend on cobalt (712% cobalt
depending on grade) as their strengthening agent. They are
cobalt strengthened 18% Ni maraging steels. Also, a new
type of maraging steel is introduced which contains no cobalt
and has titanium as a primary strengthening agent. They
are titanium strengthened 18% Ni maraging steels. Cobaltstrengthened grades, or C-type 18Ni maraging, are designated by the letter C in the grade identification and

Corresponding author. Tel.: +82 62 972 6707; fax: +82 62 972 6670.
E-mail address: opentest@kitech.re.kr (D.G. Lee).

0924-0136/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2005.02.102

titanium-strengthened grades, or T-type 18Ni maraging, are


designated by the letter T in the grade identification. The
two types of steels are classified into 200, 250, 300, and 350
grades again by their strength levels and these are named C200 or T-200, etc. It is strengthened through easy precipitation of metal compounds by aging treatment because this ultra
high tension maraging steel employs precipitated hardening
alloy elements such as Co, Mo and Ti in FeNi martensite
of 0.03% low carbon or less [4]. In early 1980s, maraging
steel which does not contain cobalt was commercialized and
named Co-free maraging because the price of cobalt was
so high.
Maraging steels are furnished in the solution annealed condition. They are very tough, relatively soft (2832 Rc) and,
therefore, readily machined and formed. They achieve full
properties through martensitic precipitation aging (hence the
name maraging steels)a relatively simple, low temperature
heat treatment. As is true of the heat treating procedures, aging is a time/temperature dependent reaction. And the steels
are so many demanded.
Excellent mechanical properties
high yield and ultimate tensile strengths;

D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

343

high toughness, ductility, and impact strengths;


high fatigue strength;
high compressive strength;
hardness and wear resistance sufficient for many tooling
applications.
Excellent heat treat treatment characteristics
low furnace temperatures required;
precipitation hardening, aging heat treatment;
uniform, predictable shrinkage during heat treatment;
minimal distortion during heat treatment;
through-hardening without quenching.
Excellent workability
easily machined;
high resistance to crack propagation;
readily formedcold, warm, or hot.
Therefore, in this study we will consider how to get better
mechanical properties such as strength and elongation more
than 250 grade though it is similar to only 200 grade by
using the condition of solution and aging treatment which
has being applied to 18% Ni maraging steel up to now. Also
according to the amount of Nb (niobium) content and aging
condition, we carry on strength test to find out an optimal
time and temperature for aging treatment and to compare and
evaluate it with test results. Therefore, we carry on practical
study applicable for the present manufacturing method which
does not need the investment of particular equipments or the
change of manufacturing process.

2. Specimens and experimental works


2.1. Material and teat-treatment
The materials used in this study was 18% Ni maraging
steel, and to analyze the effect of Nb condition and aging
treatment on the strength, the ingots which contained 0.00%,
0.03%, and 0.06% Nb were prepared with the standard chemical composition by a VIM as shown in Table 1 which shows
the test result of chemical compositions of ingot made by wet
analysis devices (Maker: METROHM), and the result is very
similar to expected alloy composition. Also in the result of
analysis by C/S concurrent analyzer (Maker: LECO), C is
0.0022 wt.% and S is 0.0007 wt.%, and it is considered that
these compositions came from the remaining air, not added
intentionally, but it did not have an effect on the strength
of steel due to extremely small quantity. We carried on hot
rolling process at seven steps for three readymade ingots,
and finally earned 12 mm rolling thickness. At the extracTable 1
Chemical compositions of manufactured maraging steels (wt.%)
Materials

Ni

Co

Mo

Al

Ti

Nb

0.00% Nb
0.03% Nb
0.06% Nb

18.03
17.96
17.98

8.42
8.39
8.43

4.99
4.94
4.96

0.10
0.09
0.10

0.41
0.39
0.40

0.000
0.033
0.068

Fig. 1. Heat treatment diagram.

tion stage, the temperature of ingot was 1225 C, and took


about 1 min for rolling process at seven steps. Table 2 shows
mechanical properties of the specimens. As shown in the table, yield strength and tensile strength are slightly increasing
0.00% Nb, 0.06% Nb, and 0.03% Nb in order, not appearing
any differences. Elongation and modulus increased in proportion to the quantity of Nb contained, and reached up to
0.06% of the highest rate.
The three aging temperatures, 455, 482, and 510, at 30 C
based on the most standard temperature 482 C were set to
study temperature and time effect on Nb contains. To find out
how the aging treatment time has an effect on the strength of
maraging steel, the maintaining time was extended to four
types of 1, 2, 4, and 8 h. Each specimen is put in the pot at set
temperature, and temperature variation during heat treatment
was kept within about 2.9 C. Cooling process was cooled up
to room temperature as the same method as solution treatment.
Figs. 1 and 2 are treatment diagrams of solution annealing
and aged hardening and outline of the experimental procedure
with test parameters briefly.
2.2. Experimental works
The samples for fabrication of test specimens were also extracted from the middle part of the pressed steel, and the specimens for tensile test were extracted so that the load direction
can be in accord with the rolling direction. Specimen preparation procedure is as below. The pressed steel, which is 12 mm
in width and 1600 mm in length, was cut by 160(W) 500(L)
to be easy to fabricate, and 2.75 mm milling fabrication was
Table 2
Mechanical properties of the three different base metals
Materials

Yield strength
(MPa)

Tensile
strength
(MPa)

Elongation
(%)

Youngs
modulus
(MPa)

0.00% Nb
0.03% Nb
0.06% Nb

892.16
900.17
894.95

980.13
986.45
982.84

21.16
21.40
23.12

8362.97
8407.56
8606.28

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D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

Fig. 2. Outline of the experimental procedure.

Fig. 3. Tensile test specimen (sub-size).

made on each side, and it became 6.5 mm in width and then


the first grinding was executed. After grinding, treat tensile
test specimens and fatigue test specimens were fabricated by
using wire discharger (wire diameter 0.2 mm). Fig. 3 illustrates the shape and size of tensile specimens manufactured
by sub-size according to ASTM E-8 [5]. The capacity of the
tester is 50 t (Fig. 4).
The samples for fabrication of fatigue test specimens were
also extracted with sufficient margin so that crack direction
can become LT direction (Long Transverse direction) [6,7]
which is rectangular to press direction, and grain boundary
can block fatigue crack frequency, and also the thickness of

top and bottom side became 10.21 and 10.4 mm in width by


cutting and grinding. The reason of this work was to consider
the effect of sliced section contraction during solution and
aging treatment, and the grinding was made 10 mm in width
after heat treatment. It was fabricated with wire discharger
(wire diameter 0.2 mm) in accordance with ASTM E647-83
[8] standard. Spare notch is fabricated at a depth of 3 mm
on the related position by using diamond wheel cutter of
0.15 mm in width. Fig. 3 illustrates the shape and size of CT
specimen for fatigue test.
Tensile test was carried out three times respectively with
load of 10 t, at crosshead speed of 3.5 mm/min and at normal temperature, and took an average. And the fatigue life
and stress intensive factor were compared with the test results. As the conditions of fatigue test, frequency is 10 Hz,
stress ratio is 0.1, frequency shape is sine curve, and all tests
were made in same method at standard temperature and under ASTM standard E647-88 regulations [9]. For the measurement of crack we set a crack gauge on the front side of
specimen to measure the displacement of open crack part, and
got the compliance from this displacement and load signal,
and converted it. In the accuracy of crack length, consider-

Fig. 4. Fatigue test specimen.

D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

345

ing of resolving ability of 12 bit A/D converter included in


the controller, the measurement accuracy of open crack part
is approximately 0.0001 mm, and when it is converted into
crack length, it is about 0.01 mm. As all processes such as
load control, crack length measure, and handling, excluding
specimen loading and unloading were programmed and automated, it is considered reliable.

3. Results and discussion


3.1. Effect on micro-structure and hardness
Fig. 5 shows the change of the Rockwell hardness value
according to the aging time. The value of the base metals
with 0.03% and 0.06% Nb had almost the same showing
that the former and the latter were about HRC 29.4 and
HRC 29.0, respectively. Also, the solution annealed specimen at 815 C for 1 h was HRC 25.128.8 which was about
3% less than base metal. Specially, the value of 1 h aged
samples highly increased more about 4763% than that of
base metal and increased in the order of aging temperature
455 C < 482 C < 510 C, showing the longer aging time and
higher aging temperature, the higher hardness value. But the
increasing rate decreased rapidly in proportion as the aging
time increases. The result was that the value at 510 C for 8 h
was lower than that of the others specimens. This result was
caused by the over aging phenomenon because the aging time
and temperature were so high that the reverse transformation
martensite was formed [10].
3.2. Effect on yield strength
Fig. 6 shows the effect of heat treatment temperature and
Nb content on the yield strength. The yield strength having
0.00% Nb was little bit low than solution annealed specimen. But it much increased after 1 h aging showing that the
longer aging time, the higher yield strength. The strength
increased in order 455 C < 482 C < 510 C at 1, 2, 4 h aging respectably showing that the discrepancy in strength was
going from 1 to 4 h, it showed almost same strength at 8 h
regardless of aging temperature at last. These results could
be analyzed and had a good agreement that the higher aging
temperature, the shorter aging time, and the aged strength
decreased at high temperature and over suitable time on the
contrary [11,12]. The overall tendency in case of 0.03% and
0.06% Nb specimen was similar to the 0.00% Nb content
showing that tensile and yield strength was lowest at 510 C
for 8 h caused by the over aging. Collating these various results, the solution annealing at 815 C for 1 h had no effect
on the strength. But the strength increased about 450, 550,
580 MPa at 455, 482, 510 C respectably. The most excellent aging condition was 8 h aged at 482 C with 0.06% Nb
content showing that the strength of the specimen increased
twice more than that of the base metal. Elongation rapidly
decreased at 1 h aging and then it was slowly decreased as

Fig. 5. Effect of Nb content and aging temperature on the Rockwell hardness.

seen in Fig. 6(c). The most excellent condition for elongation


was 0.03% Nb material aged at 455 C for 1 h having about
97% of base metal. SEM micrographs for 0.03% Nb specimen as seen in Fig. 7 showed some dimples generated by
micro-voids [13,14]. At 455 C for 4 h, 482 C for 2 h, and
510 C for 1 h, the dimples showed maximum numbers and
minimum size.
3.3. Effect on fatigue life
Fig. 8 indicates aN diagram of base metal before heat
treatment which contains 0.00%, 0.03%, and 0.06% Nb and
a test specimen, of which the mixture treatment has completed for 1 h at 815 C. It is a representative diagram which

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D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

Fig. 6. Effect of Nb content and aging temperature on the yield strength and elongation.

indicates the relation of fatigue crack length and the number


of cycles. Reviewing the fatigue life of base metal with no
heat treatment, the fatigue lives of specimens of 0.03% Nb
and 0.06% Nb are very similar, but increased about 4% more
than 0.00% Nb. Therefore in case of base metal, the fatigue
lives not much influenced by change of Nb quantity. However, in the solution annealed specimen as shown in Fig. 9,
the fatigue life of specimen to which Nb is added is approximately 6% lower than specimen to which Nb is not added
and the life increases 0.06% Nb, 0.03% Nb and 0.00% Nb
in order. Therefore, Nb addition on mixture treatment may
reduce fatigue life. In conclusion, if we compare the fatigue
life of solution annealed specimen at 815 C for an hour and

that of base metal not treated, the fatigue life of specimen


to which Nb is added increases more than Nb base metal,
but the fatigue life of solution annealed specimen decreases.
Therefore mixture treatment decreases the fatigue life, as Nb
increases from 0.03% to 0.06%, the fatigue life decreases
more or less.
Fig. 10ac shows the relation between aging time and fatigue life of each Nb contained specimen to analyze effect of
aging time on fatigue life, and compare between aging treated
specimens. The effect of aging temperature on fatigue life of
0.00% Nb specimen, the life increases as increase of aging
temperature such as 455, 482, and 510 C. At the same aging temperature, the longer aging time the longer fatigue life.

D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

347

Fig. 7. Fracture surface of tensile test specimen.

Fig. 8. aN diagram of base metal specimens.

Fig. 9. aN diagram of solution annealed specimens.

However, if we look at 455, 482 and 510, 455 and 482 C are
nearly linear increase but for 510 C, increase rate is slowdown at 4 and 8 h area. The cause of this situation is that; it is
necessary to treat longer time at lower temperature to do aging
treatment of maraging steel, shorter time at higher temperature. If aging time is unnecessarily long reverse transformed
martensite is formed, and it is cause of strength and fatigue
life reduce. As shown in figure of the 0.03% Nb contained
specimen, the higher aging temperature, the longer fatigue
life is, and at the same temperature, the longer aging time is,
the longer fatigue life is. Fatigue life increase rate deviation
between 4 and 8 h is only 2% at high temperature, 510 C.
But the life increase rate deviation is 30% between 4 and
8 h at 455 C, which is the highest increase among the test
temperatures. This reason is that aging for 8 h at 510 C is
over-aging. In case of 0.06% specimen, the effect of aging
temperature on fatigue life is same. Also, increase of fatigue
life at 510 C is same. The longer aging time at high temperature is, the slower fatigue life is. Refer to above study
we can find an effect of aging temperature on fatigue life.
In the fatigue life at 455 C, the more aging time increase,
the more it increases is linear. However, in aging treatment
at 482 and 510 C, it increases nearly linear up to 4 h and
slow down after 4 h. Particularly the fatigue life increase rate
over 4 h is very low at 510 C due to over-aging and formation of reverse transformed martensite [15,16]. Because we
achieved this study within optimal aging temperature interval
of 18% Ni maraging steel, so the higher aging temperature
the longer fatigue life. Remarkable life reducing due to over
aging was not found, but life reduction may occur with aging

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D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

Fig. 10. Effect of aging temperature on the fatigue life.

Fig. 11. Representative fatigue fracture surfaces. The crack has grown from left to right.

for 8 h or more. A special feature remains on the fracture


surface of materials, and it is useful to investigate the cause
and mechanism of fracture. Fig. 11 representatively shows
the fracture surface to obtain a better understanding of the
failure micro-mechanism. The pictures show the surface on
0.6 mm distance position away from the end of crack initiated
point. All of the specimens clearly were brittle similarly.

4. Conclusion
Effects of niobium contents and aging conditions on the
strength and fatigue life of 18% Ni maraging steel commonly
using in aircraft, space field, nuclear energy, and vehicle, etc.
were investigated. Three different niobium contents, 0.03%,
0.03%, and 0.06%, three aging temperatures, 455, 482, and

D.G. Lee et al. / Journal of Materials Processing Technology 162163 (2005) 342349

510 C, and four different aging times, 1, 2, 4, and 8 h at those


temperature respectively were the parameters for hardness,
tensile, and fatigue test.
(1) Hardness value decreased about 3% for annealed specimens and increased about 60% for 1 h aged specimens.
But the values of the other specimens aged 2 h or more
showed almost the same.
(2) The yield strength was the highest about 1800 MPa in
0.06% Nb specimen having twice as much as the base
metal specimen. Also, the elongation was the highest
in 0.03% Nb specimen showing the same as base metal
specimen.
(3) In result of fatigue test, it showed that the higher aging
temperature and the longer aging time, the higher fatigue
life. On the other hand, the 0.03% Nb specimen showed
the highest fatigue life which increased about 12% more
than base metal specimen.
(4) 0.06% Nb specimen aged at 482 C for 8 h simultaneously satisfied the 250 grade strength and 200 grade elongation having the most superior mechanical properties.

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