Академический Документы
Профессиональный Документы
Культура Документы
Center,
of Mechanical Engineering,
Abstract
X-ray stress constants
H13) were
by
diffraction peak using Cr-K, radiation, and for specimen I3 (E - FesN and y-FedN, treated at 833K
for 30h) was KB = -920 MPa/deg.
(2) Nitriding
specimens
showed
a decrease
of heating resistance
of the
nitriding layer during the heating test. The oxidation of the nitriding layer began at 723K (450C) as
examined by measuring weight, X-ray diffraction profiles and by microphotographic
observations.
1. Introduction
Die casting dies and forging dies are considerably
repetitions of heating and cooling). One of the ways to increase the life of a die is to use a nitriding
process, such as gas-nitriding,
carbo-nitriding,
in industrial products.
After the nitriding process is applied to a hot working
thermal fatigue characteristics
However,
surface2).
Thermal
fatigue behaviour
of nitriding
hot working
by
measuring residual stress using a Fe 211 diffraction with Cr-K, radiation including the peaks of Fe-N
compounds,
and by observation
However,
compound
concerning
the phenomena
of Fe-N
so far 4,5)
in the
heating
microphotographic
test
by
measuring
the
cycle) by measurements
the decomposition
weight,
X-ray
and oxidation
diffraction
in
of X-ray
of nitriding
profiles
and
by
observations.
2.
Experimental
2.1
Determination
procedure
of X-ray stress constants
Specimens used are shown in Table 1. The specimens were machined by means of grinding.
Before the nitriding process, specimen B was heat treated at 923K(650C)
Fe4N. Also, a Fe was identified. For the specimen B, the nitrides were E -Fez_sN, E -Fe3N and y Fe4N. Fez03 was formed during the stress release heat treatment.
From the results of identification for specimen A, E -Fez_sN 103 diffraction by Cr-K, radiation
was used. The peak position
was about
diffraction with the same radiation was used. The apparatus for X-ray stress measurement
RIGAKU
MSF-2M
system
and w -goniometer.
was a
There
are two cards for Centre
&-phase
(No.Data
30925
and No. 11236) in the JCPDS file and both of them are described
Copyright *(C)
JCPDS-International
fornitride
Diffraction
1997
as Fe3N. However, the card No. 30925, had been described as Fe2_3N.In this study, in order to differentiate one from
the other, the card No. 30925 is described as Fe2_3N,and No. 11236 as Fe3N.
Also, an R -
constants were obtained from change of slope of 2 0 -sir? v diagrams. A strain gauge was attached
to the tension
specimens
Especially, in case of the 103 diffraction for the specimen A and the 200 diffraction for the specimen
B, a strain value of 1OOOxlO-6was added.
five times.
Applied stresses in this experiment were calculated using the Youngs modulus for H13
(208.8 GPa). The values of sin* w in the diagram were from 0 to 0.6 with an interval of 0.1.
Table1 Specimens
Specimen
Material
Width-length-thickness,mm
Nitriding condition
SKD61)
10-100 -3
Quenching and tempering
,45 HRC
833K(560C),30h
843K(570C),6h
600
P
g 400
E
40
60
-40
80
Diffraction angle,
28
(deg.1
60
80
100
Diffraction angle, 2 e
120
140
160
(deg.)
were prepared
from hot working die steel (AISI H13, JIS SKD61) which was heat treated and hardness of 48HRC
was obtained.
hours.
In the thermal fatigue test, the specimen was heated up to 843K (570C) for 160sec. by
contact to a heating block, and was cooled to 373K ( 100C) in a water bath. Heating temperatures
are representative
was -648MPaldeg.
with Cr-K,
Also, the peak at about 156deg. which was diffracted from both the E - Fez_jN
200 and the a Fe 211 was used with the X-ray stress constant (-297MPa/deg.)
Diffraction angle,
28
(deg.)
Fig. 2 X-ray diffraction profile of specimen for the thermal fatigue test
2.3 Phenomena
Specimens were heat treated to 45HRC and prepared by wire EDM (15mm width, 25mm
length and 0.5mm thickness).
were heated from 673K to 973K, for each 50K, they were kept 6 hours then
= w;WQ
0
x 100
(%)
(1)
Copyright where
(C) JCPDS-International
for Diffraction
1997 before and after heating.
W0 and WT are Centre
the weight
of the Data
specimen
Copvrinht 0 JCPDS-International
of
Fig,3 shows the CJx-M and CJx-2 8 V=~diagrams obtained from each specimen, where M is the
slope of the 2 0 -sin2 w diagram, 2 8 ,+,=ois the intercept, and o x is the applied stress.
the diagram of specimen B for the E - FesN 103 diffraction were somewhat scattered.
other results:
The plots in
However, the
E Fe2_3N 103 diffraction for specimen A and E -FesN 200 diffraction for specimen B
is more accurate
Stress measurement
103 diffraction.
In case of the
of the X-ray stress constant of the E -FejN where the 103 diffraction peak overlaps the
APPII~
,._
stress,o r (MW
-P -0.10
3
r
g -0.20
0
B
3
5 -0.30
ii
..:.....
r ........
162.8
pzh,,,i
.............!
_.._
/2Ip
L....
.................
,
..,+
&.
..........
j.. ............
;/; i
A*::.
: .....
...... i.. ........... . ...... ;_.
j
....
i..
...........
... .
I- ...
50
150
162.7
e
3
50
100
150
200
250182.6
200
(MPa)
(c)
8
2
S
d
t
Applied stress, a y
CowriaRtO JCPDS-International
t3
.: ..
0
100
162.8
i ..
5 -0.40
0
(MPa)
diagrams
The values of X-ray stress and elastic constants obtained from these figures and the residual
stresses are shown in Table 2.
compressive
The confidence
in specimen A.
It is found that
obtained.
Table 2
=--.
s, L-E
828,
3 (.Tx
.-
dM
2(1w)
. a
fjo
s,
=--
--
18)
r
*-
3 (J x
a% &
1%)
had a
The intensity of this diffraction peak began to decrease at 50 cycles and disappeared
at 500 cycles.
On the other hand, before 20 cycles, the residual stresses obtained from the peak at 156 deg.
namely the E -Fez_sN 200 diffraction with the a Fe 211 showed the same results as the E -Fe2_3N 103
diffraction.
At 50 cycles and 100 cycles, it was observed that the residual stress tended to decrease
and was scattered widely. After 200 cycles, the residual stress fell in the range of about -200 to
-4OOMPa. The value of the peak intensity increased 2 times at 1000 cycles, however, that of the E Fe2.3N 103 diffraction
decreased
between
peak didnt
decreased
The
peak
around 156 deg. fell off to nearly 3.3 deg. which is the value for quenched and tempered die steel.
From the results
peak intensity
Copyright (C) JCPDS-International
Centreofforresidual
Diffractionstress,
Data 1997
at
around 10 to 20 cycles some changes were begun to be observed in values from both the E -Fe2_3N
peaks.
In the range from 100 to 500 cycles, major inflection points exist in
these phenomena
correspond
to decomposition
of nitrides in the 5 to 10
might cause
the change of the values and the wide scatter. For the overlapped peak, more crystallization of the
a- Fe 211 diffraction might stabilize the values in the range over 500 cycles.
processes applied to dies, during thermal cycling (heating-cooling),
In case of nitriding
what the condition of the nitriding layer is. It became clear that X-ray stress measurement
using the
peak from the E -Fez_sN 103 diffraction and the a Fe 211 with the E -Fez_sN 200 diffraction would be
one of the useful methods of quality control.
to be separated.
Also, the peak separation and the influence on residual stress of the decomposition
+Fe,,N2OO+aFe211
100
10
Number of cycles, Nf (cycle)
1000
I. ..I
-+-FeJ4
.
2OO+aFe211
103
10
. ...I
* . !
1
i...."".'._'.~""......~
,
100
1000
Fig.6
Cnnvrinht Q .ICPiI.~lntt=mdionA
1000
_f_._.__._
-a--h,$J
100
10
~~
~~~~~~
--
TqplEr
Temp. I
700
600
500
400
80
60
40
100
120
140
160
1.
1.
100
150
1.
250
300
200
50
In this
figure, the result for the specimen before heating is shown with 0 mark.
Hardness
at heating
temperature
however,
it
of nitrides
Also, the decrease below the nitride layer was due to the effect of tempering
and
decreased
furthermore,
it decreased
in the
range from the surface to a depth of about 50 pm. At 973K(700C), the hardness fell about 500 to
550 HV in all of the range, because of the influences of vigorous decomposition
X-ray microanalyzer
about 16%.
@MA) results are shown in Fig. 10. Nitrogen content of the nitride layer was
Because of this the nitride is similar to the one formed by the tufRriding process)
Before heating, the high nitrogen content area was observed to be about 40 urn. Below this
area, it decreased with the distance from the surface, and became equal to the matrix at about 250
urn. After heating at 873K (6OOC), a high oxygen content
of oxide was
observed in the region near the surface. On the other hand, the distribution curve of nitrogen content
had a convex shape. This curve corresponded
to that of nitrogen.
Copyright@ JCPDS-International
100
200
300
/L m
p m
of
layer.
400
500
600
700
Temperature, T (c)
This specimen
because
of the surface
of oxide on the surface, an increase of the weight ratio for the die steel specimen was not observed
Copyright (C) JCPDS-International Centre for Diffraction Data 1997
On the other hand, an increase of the weight ratio for the nitride specimen
was observed
In the nitriding
process,
of chromium,
Cr), decompose
of the specimen
enlargement
binds to nitrogen
is decreased.
in
in the
At high temperature,
chromium
atoms are
a nitriding process, as in
this experiment, applied to a die casting die, is able to be one of the useful methods of increasing die
life such as the reduction of the maximum temperature
4. Conclusion
Determination
processes
fatigue behaviour
has been
investigated by thermal fatigue tests and the heating tests. The results obtained were as follows:
0)
of nitriding
specimen
at 843K
peak of Cr-K,
and
specimen B (E -FesN and y-FedN, treated at 833K for 30h) was Kn = -920 MPa/deg. with
the E -FesN 103 diffraction peak of Cr-K,.
(2)
In the thermal fatigue test, however, peak intensity from the E -Fez_sN diffraction decreased
with the number of the thermal cycles and disappeared
Fez_sN with the a Fe around 156 deg. increased with the number of the cycles.
(3)
Nitriding specimens
as
examined
microphotographic
by
due to decomposition
of the
measuring
weight,
X-ray
diffraction
profiles
and
by
observations.
Acknowledgments
We thank
University for X-
References
1)
M. Hihara
and Y. Mukoyama,
Engineering,
2)
International
Journal
of The Japan
Society
for Precision
A. Schindler, A. Kulmberg and J.H. Stuhl, 9th Society of Die Casting Engineers Congress, GT77-065 (1977).
3)
Vo1.57,
4) K. Tanaka, G.Q. Ping, T. Mikuriya, Y. Akiniwa, Proc. of the 3 1st Workshop on X-ray Studies
of Mechanical
Behaviour
Japanese).
5) M. A.J. Somers and E. J. Mittemeijer, Metallurgical Transactions. A,2 1A, 189, (1990).
6)
(1994)(In Japanese).
7)
8)
M. Hihara, Y. Mukoyama and I. Ogata, Journal of The Japan Society for Precision Eng. Vo1.56,
No.8, 1508 (1990)(In Japanese).
A,21A,901, (1990).