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Pure titanium and titanium alloys have the disadvantages of a high coefficient of friction and poor wear
resistance 1. In order to improve such tribological
properties, a variety of surface engineering techniques
have been successfully applied ~-7. Of these techniques,
gas nitriding is considered to be the most promising
method available for engineering applications because
it can easily form a harder nitriding layer on the
surface of the materials. By this method substantial
improvement in wear resistance can be achieved ~-3,5,
but the fatigue strength and fracture mechanism of
nitrided materials have not been clarified.
Recently the authors have studied the fatigue
behaviour of nitrided materials based on a pure
titanium and have indicated that the fatigue strength
was improved by gas nitriding compared with the
corresponding annealed materials 8. For widespread
applications of nitriding to critical machine components, it is necessary to investigate systematically the
fatigue behaviour of nitrided materials of titanium
alloys.
In the present study, rotating bending fatigue
tests were conducted on Ti-6A1-4V alloy and T i 15Mo-5Zr-3A1 alloy, which were nitrided at 850 C
and 750 C respectively for given nitriding periods.
The fatigue strengths obtained were compared with
those of the annealed or untreated materials. Based
on detailed observations of crack initiation, crack
growth and fracture surfaces, the effect of gas nitriding
on fatigue behaviour is discussed.
0142-1123/94/060370-07
1994 Butterworth-HeinemannLtd
M A T E R I A L S AND P R O C E D U R E S
The materials used are T i - 6 A I - 4 V alloy and
T i - 1 5 M o - 5 Z r - 3 A I alloy. Their chemical compositions
are listed in Table 1.
The nitrided layers can be much deeper with
increasing nitriding temperature. However, nitriding
at higher temperatures, in particular above the transformation temperature, should be avoided because
remarkable grain growth in the core material takes
place during the nitriding process 8. In this study,
therefore, 850 C for T i - 6 A I - 4 V and 750 C for
T i - 1 5 M o - 5 Z r - 3 A 1 were used as nitriding temperatures, and thus the depth of the nitrided layer was
controlled by varying the nitriding period. Nitriding
was performed in an electric furnace, which was
evacuated before heating up to nitriding temperatures;
then nitrogen gas with a purity of 99.99% was admitted
into it. Specimens were maintained for a given nitriding
period under a constant nitrogen gas pressure of
0.13 MPa. Prior to fatigue tests, the depth of the
obtained nitrided layers was examined by hardness
measurements, and is shown in Figure 1 as a function
of nitriding period. As can be seen from the figure,
the nitrided layers become deeper with increasing
nitriding period. Similar results have been reported
for pure titanium by Yoshida and Isono z and for
Ti-SAI-2.5Sn by Mitchell and Brotherton 5. From the
results of Figure 1, nitriding periods of 4 h and 15 h
for
Ti-6AI-4V
and
20 h
and
60 h
for
T i - 1 5 M o - 5 Z r - 3 A I were chosen.
AI
6.27
3.01
4.27
Mo
Zr
Fe
Ti
0.185
0.114
0.003
0.0045
<0.001
5.05
0.206
0.042
0.015
14.51
0.0055
<0.001
bal.
bal.
80
Ti-6AI-4V alloy
Nitriding temperature
60
~ 40
"0
"6 20
-
EXPERIMENTAL RESULTS
IIIill]
10
Time
20
15
T h
E 250
200
15o
"O
100
e-
//
"6
50
"~
e..6)
Nitr'~'ng temperature
750~
/
I
10
20
30
40
Time
50
60
70
b
Figure 1 Variations of depth of nitrided layer with nitriding period:
(a) T i - 6 A I - 4 V ; (b) T i - 1 5 M o - 5 Z r - 3 A l
Fatigue strength
The S-N diagrams are shown in Figure 5 and the
fatigue limits obtained are listed in Table 3. In
Ti-6A1-4V, the fatigue strength of the annealed
materials is independent of annealing period. It is
found that the fatigue lives of the 4 h nitrided material
(N4) are shorter than those of the corresponding
annealed material (A4), but the fatigue limit is slightly
increased. In contrast, the fatigue strength of the 15 h
nitrided material (N15) is reduced compared with the
annealed material (A15) and is lower than that of the
4 h nitrided material, indicating that the harder, deeper
nitrided layer has a detrimental effect on the fatigue
strength. Similar results are obtained in Ti15Mo-5Zr-3AI alloy: the fatigue strength of the 20 h
nitrided material (N20) is decreased compared with
the annealed material (A20), while the fatigue lives
of the 60 h nitrided material (N60) are shorter than
those of the annealed material (A60), but the fatigue
Fatigue, 1994, Vol 16, August
371
Mechanical properties
Alloys
Ti-6AI-4V
Ti-15Mo-5Zr-3AI
Treatment
0.2%
proof
stress, cro2
(MPa)
Tensile
strength, crB
(MPa)
Breaking
strength
on final
area, ~rT
(MPa)
STA
A4
N4
A15
NI5
1132
927
890
900
925
1238
971
943
950
974
1518
1365
1206
1320
1338
A20
N20
A60
N60
957
871
975
875
1015
916
1001
901
1923
1671
1941
1579
Elongation, ~b
(%)
Reduction
of area,
(%)
9
7
40
49
40
48
45
11
7
13
13
41
46
40
47
11
13
12
4~
Ti-6AI-4V alloy
~g
"1-
N4
"l-
N9
U~
[] N15
t-
N20
t~
tN_
E
o
z
1
0
50
100
150
/1 m
2.4
Ti-15Mo-5Zr-3AI alloy
2.2
-1-
,~]~
"~
"1- 2.0]
0 N4
/ ~
Figure 3 Microstructures of nitrided Ti- 15Mo-5Zr-3AI: (a) nitriding for 20 h (N20); (b) nitriding for 60 h (N60)
a)
c
t"-
1.8
1.6
.20
,\ \
[].,o
%\
x~ 1.4
.__
.e 1.2
o
z
1.0
0.~
50
100
150
200
250
Distance from surface d /~ m
300
b
Hardness profiles of nitrided materials: (a) Ti-6AI-4V;
(b) Ti-15Mo-5Zr-3AI
Figure 4
m 800
o-=
700
2pm
"10
Ti-6AI-4V allOy
Rotatingbending
o =570MPa (R=-1)
ZXA4
t.'~. %
t~
O4
4/zm
T
!
|
N15
Surface removal
for N15/(5/Jm) ~
a.
E 60G
_]
L..
O
~ 500
N15
Surfaceremovalfor N15
400
i
, ,,.,,I
.,,.,,I
10 4
103
00
i
. ,,,,,I
10 5
,.i.,
10 7
10 6
Nf
3
4
5
6
7
Number of cycles N 104
800
Ti-15Mo-5Zr-3AI alloy
Rotatingbending
(R=-I)
~; 700
O
[]
600
E
E 7
A20
A60
N20
N60
500
(3---*
t~
400
82
g
.....
10 4
. . . . . .
10 s
,a,,,,l
. . . . . . .
10 6
10 7
A20
N20
A60
N60
j,
1
Number of cycles
Nf
104
b
Figure 5
Table
[]
Ti-15Mo-5Zr-3AI alloy
Rotating bending
o =500MPa
(R=-I)
S-N
3 Fatiguelimits
Alloy
Ti-6AI-4V
Yi-15Mo-5Zr-3Al
Treatment
Fatigue limit, Cw
(MPa)
STA
A4
N4
A15
A20
N20
A60
N60
720
510
555
490
450
375
350
375
373
p.m)
is shown in Figure 7. It can be seen from the figure
that the crack reached the core material, but its depth
a is only 133/zm; thus the aspect ratio a/c is extremely
small. The same phenomenon was observed in
Ti-15Mo-5Zr-3A1. These observations suggest that a
crack is initiated suddenly at a relatively large size or
grows rapidly in the surface layer. As this crack grew
into the core material and led to the final fracture,
premature crack initiation is primarily responsible for
the reduction in fatigue strength for the nitrided
materials.
There was a considerable difference in crack morphology on the specimen surface between the annealed
and nitrided materials. Cracks in the annealed materials
exhibit an extremely tortuous path due to the effect
of microstructure, while cracks in the nitrided materials
reveal a straight morphology without any deflections.
SEM fractography
As a typical example, SEM images of the fracture
surfaces in Ti-15Mo-5Zr-3AI are shown in Figure
10. There is a clear difference between the nitrided
and annealed materials. In the annealed material,
radial markings from the crack initiation site are
observed and thus the crack is considered to grow
concentrically. In the nitrided material, markings
perpendicular to the specimen surface are observed,
indicating that the crack suddenly initiated at a
relatively large size and grew into the bulk. These
features in SEM appearance of the fracture surfaces
were also obtained in Ti-6A1-4V.
DISCUSSION
1.0
o
o
"~
0.8
0.6
1)
~ 0.4
/
0.2
zx A4
[] A15
,J
---"
N15
10
374
between
aspect
ratio and s u r f a c e
crack
(9
~ 10-2
E
E
z
10-3
Ti-6AI-4V alloy
Rotating bending (R=-I)
cr =570MPa
zx
[]
A4
N4
A15
N15
Surface removal
for N15 (51z m)
(9
10-;
E
E
z"10 10-3
. . []
Ti-6AI-4V alloy
Rotating bending (R=-I)
cr =570MPa
A A4
N4
[] A15
N15
O Surface removal
for N15 (5/z m)
r-~
(9
10-4
t-
10 -5
0
"#
Ill
(9
10-4
t-"
,,,,,I
,,,,,I
[]
10-6
,,,,,
0.5 1
5 10
50
Maximum stress intensity factor
(Kmax)A MPa~m
C~
10-5
[]
10-~).
r-l
0.
i i nil
* * I 111
I i i
0,5 1
5 10
50
Maximum stress intensityfactor
(Kmax)C MPa~m
Figure 9 Crack growth behaviour in Ti-6AI-4V: (a) specimen surface; (b) deepest point
.........
5a).
375
ACKNOWLEDGEMENTS
The authors wish to thank H. Sekiya, Y. Matsunaga
and C. Asahara for the nitriding treatment performed
in Gifu Prefectural Metal Research Institute. Thanks
are also due to Y. Kamiya and G. Hisamatsu for
assistance with the experiments.
REFERENCES
1
2
3
4
5
6
7
8
9