Effect of Repeated Nitriding on Aluminum

Die casting Die Surface and their Die Life

Masahiko Hihara ,Koji Yatsushiro
Yamanashi Industrial Technology Center,
Yamanashi, Kofu, Japan

The die surface of hot work die steel(JIS-SKD61,AISI-H13),

as used aluminum die casting die, is loaded with thermal
stress, causing thermal fatigue induced by repetitive heating
and cooling. The excessive load gradually shortens the life up
of die surface (cavities).
In the recently years, surface of aluminum die casting die ,
forging and extrusion dies are treated with various nitriding
processes to stabilize the die cast, improve its performance
and life up. The nitriding process has proven to increase the
heat-checking resistance on the hot work die steel, thus greatly
reducing the maximum crack length on the nitrided SKD61,
compared to the non-nitrided SKD61.
It is reported that, heat-checking resistance caused minimal
amount of nitride(refereed to as white layer) such as e
phaseFe2-3Nand g phase(Fe4N). The maximum surface hardness
after nitrided process was 800HV , and furthermore, it
was note that, compared to non-nitrided die, nitrided die
steel specimens with hardened layer achieving 100 to 150m
showed superior results.
Seldom a production is completed with a single nitriding
treatment. For prolonged productions, several nitriding
process is repeated during production in order to maintain the
quality of die surface and to extend the life up.
The advantages of repeated nitriding process are, (1) increase
of compressive stress and recovery of damaged surface, (2)
maintaining a stable surface quality throughout the productions
usage. However there are very few reports clearly discussing
these advantageous points.
In this study, repeated peening and nitriding treatment
was conducted 1 to 3 times using the improved SKD61
specimen for the purpose of identifying thermal fatigue on
the nitrided surface.
This report presents the study results of residual stress of
treated nitrided surface (SKD61), measured by X-ray residual
stress method, observation of decomposition in nitride and
diffusion layers, and changes in measured hardness and residual
stress of into the sectional area of the tested specimen.

Experimental procedure

1. Material

Material used in this experiment is improved hot work die steel.

The basic compositions of this alloys are, 5%Cr-2.5%Mo-1%V.
Characteristics are improved toughness, adhesion resistance
and hardenability. The dimensions of machined thermal fatigue
testing specimen, made from cylindrical bar are; 58 mm
diameter, 20 mm thickness as shown in Figure 1.
Thermal stress was loaded to the specimen surface by repeated

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Yoichi Nosaka

MITSUI MINING & SMELTING CO.LTD,Yamanashi,

Nirasaki, Japan

Fig. 1 Specimen shape for thermal fatigue test

heating - cooling process during thermal fatigue test underwent

emery polishing, followed by quenching and tempering treatment
by thermal flow as shown in Figure 2. The surface hardness
achieved by this thermal treatment was 48HRC.

2. Peening and gas-nitriding treatment

Figure 3 shows repetitional conditions of peening and gas-

Fig. 2 Conditions of thermal treatment

nitriding treatments. Peening treatment was carried out before
and after gas-nitriding treatment. In order to develop structure
refinement of the metal surface prior to the treatment, an
approximate diameter of 100 mm carborundum particles
was employed to obtain an evenly processed homogenized
surface.
After the nitriding process, oxide layer formed during this
process was removed, and the surface was polished by peening
treatment using glass beads with approximate diameter of 30 to
50 mm to develop the thermal fatigue testing specimen.
Second and third treatments of the specimen was conducted
following the same conditions as set forth in the first peening

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Fig. 3 Conditions of peening and nitriding treatment

and gas-nitriding treatment. For discussion purpose, the
treated specimens shall be identified as A,B and C, in the
order of the treatment.

3. Thermal fatigue test

The thermal fatigue test was conducted by using the same

Fig. 5 X-ray diffraction profiles as treated specimens A ,B and C

(peening and nitriding treatment)

Fig. 4 Schematic view of thermal fatigue testing apparatus

testing apparatus shown in Figure 4. The specimen surface was

heated to 570 for 160 sec. by means of thermal transfer, then
dipped 5 mm of the heated surface in room temperature water
for 15 sec. to cool the surface to 100.

4. X-ray residual stress measurement

The residual stress measurement and observation of X-ray
diffraction profile in this experiment used Cr target with
Cr-Ka characteristics. The X-ray diffraction profile of specimens
A, B and C are shown in Figure 5. In observing the diffraction
profile, it clearly evidenced the diffraction line of Fe211.
Therefore, this diffraction line was used, following the
conditions set forth in Table 1 to conduct the X-ray residual

Fig. 6 Micro-photographic observations of sectional area for the

specimen before the thermal fatigue test
stress measurement (The apparatus used for this experiment
was Rigakus MSF-2M)
Residual stress measurement of the specimen surface and
sectional area after the thermal fatigue test was obtained with
measuring positions shown in Figure 1. The designated space
for the test was set at 15 mm from the specimen surface edge
with an area of 5x5 mm. An average value obtained from
four points of equal distance was employed to determine the
residual stress measurement.
The residual stresses measurement for the specimen depth
followed the same procedure as discussed above, testing

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each surface layer by removing it with electrical polishing

method. Thus, the cracks and residual stress were measured
from the position.

Experimental Results

1. Observations of gas-nitrided layer

Figure 6 presents the micro-photographic observation of

sectional area prior to thermal fatigue testing of repeated gasnitrided specimen A, B and C. Nitride layer(white area shown
in the photograph) was minimally observed on the surface
of specimen A, due to gradual thickening of nitride layer as

Repeated micro-photographic observation was made by

buff polishing the surface until most of the oxided layer was
removed and slight heat-checking was detected. The width of
the crack diminished with the repeated nitriding process and
a fine network was formed. Observing the sectional area of
specimens A, B and C, the oxided layer slightly increased it
thickness as nitriding was repeated.
In the case of non-nitriding specimen, heat-checking formed
during thermal fatigue test gradually penetrated into the matrix
from the surface. However, in the case of the three nitrided
SKD61 specimens, A, B and C, the cracking did not occur
beyond the diffusion layer as can be observed in the center
bottom of the photograph (dark colored layer). It is therefore
considered that diffusion layer by nitriding inhibited further
crack growth.

2. Hardness measurement

Fig. 7 Micro-photographic observations for surface and sectional

area of the specimens before and after the thermal fatigue test
surface (a) above and sectional area (b) below

the process was repeated. However, specimen C evidenced a

thin but uniformed nitride layer due to 3 times of nitriding
processes. It is considered that the increased nitride developed
from repeated nitriding process is due to following the same
condition for each treatment.
Observing the diffusion layer of each specimen, the depth was
almost the same for every treatment process and therefore, no
apparent structure difference was found. Micro-photographic
observations of the surface and sectional area after the 1.5x104
cycles thermal fatigue test for these specimens are shown
in Figure 7. Clear observation of heat-checking (crack) is
difficult due to the oxided layer formed on the surface after
the test.

Fig. 8 Vickers hardness distribution curves of the Peened and

nitrided specimens and used die

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Figure 8 shows the hardness distribution curves of gas-nitrided

specimens for the sectional area before and after 1.5x104
cycles test. The maximum hardness value of specimen A was
approximately 680HV prior to treating the surface, similar to
the diffusion layer with minimal nitrided layer. However, in
the case of specimens B and C, because nitrided process was
repeated 2 and 3 times respectively, compared to specimen A,
the surface hardness showed a higher value of 830 to 850HV.
It was considered that the higher hardness value in specimens B
and C was due to the precipitated nitride in the grain boundary
under the nitride layer.
Furthermore, comparing the hardness of each specimens at
a depth of 20 to 40 mm from the surface where there is no
nitride, clear value difference was observed between the single
nitrided processed specimen A and specimens B and C where
nitrided process was repeated 2 to 3 times.
For reference purpose, the results of hardness measurement
prior to using the die treated 7 times for peening and gasnitriding is also shown in Figure 8. In this case, the hardness
value of the die surface greatly increased to 1100 HV. The
hardness layer was also shown to increase its depth. This seems
to indicate the possibility of increasing the surface hardness
depth by repeating the nitriding process.
However, in this experiment, the difference in the hardness
layer depth was not clearly defined between the 3 specimens.
Therefore, it may be concluded, as mentioned earlier, that
in the case of specimens B and C, surface hardness is greatly

Fig. 9 Relationship between number of cycles to residual

stress
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dependent on gas-nitriding with very little affect on the depth

of the diffusion layer. The surface hardness of each specimen
was measured after the 1.5x104 cycles thermal fatigue test. The
surface hardness decreased due to its reaction to heat. The
hardness reducing value for specimen A was 100HV and 200
to 260HV for specimens B and C.

3. Residual stress measurement

Observing the X-ray diffraction line profile shown in Figure 5,

the peak intensity increased in low angle Fe2-3N002 diffraction
and Fe2-3N100 diffraction. Therefore, even for specimen C
where nitrided layer Fe211 diffraction was considered to be

thick, the broadening was insignificant compared to other

specimens. Somers et al reported that thickness of nitrided layer
will increase with increased nitriding treatment temperature
and increased NH3 gas atmosphere. The reason was due to
minimal removal of the hard nitride surface caused by peening
treatment for each step.
Figure 9 shows the relationship between number of cycles to
residual stress. Fe211 diffraction line included with Fe2-3N200
diffraction line was used to measure the residual stress.
The surface residual stress for specimen A showed a large
compressive stress of approximately -1.0GPa before the test.
The residual stress value gradually decreased with increased
testing cycles, further decreasing beyond 103 cycles, achieving
the same value of 400MPa along with specimens B and C
at 104 cycles.
The residual stress on the surface of the specimens B and C
before the test showed a compressive stress of approximately
-700MPa. Each specimen showed the same tendency of
compressive stress decrease. However, specimen A showed
a greater compressive stress during the early cycles ranging

Fig. 10 Residual stress distribution curves of the Peened and

nitrided specimens and used die

Fig. 11 Results of crack measurement for after thermal fatigue

tested specimen
from 1 to 103 cycles.
Many cracks evidenced in each specimens residual stress
surface at the level of 1x104 cycles. Therefore, it is considered
that since the existence of the cracks released the thermal
fatigue damage and the residual stress value, measured residual
stress has the same value for each specimen.
Figure 10 shows the residual stress distribution curves
for gas-nitriding specimen A, before and after testing the
sectional area with the 1.5x104 cycles test. The comprehensive
stress of the surface showed approximately -1.0GPa.These
values gradually decreased, increasing the distance from the
surface. The stress existence depth value at the matrix was
approximately 80 mm.
On the other hand, the surface residual stress for specimens
B and C was in the range of -700 to -800MPa, which was
200 to 300MPa less than specimen A. We believe the reason
for this difference is due to effect of residual stress on the
behavior of the nitrided surface caused by an increase due
to nitride layer which formed near the surface by repeated
nitriding process.
Maximum residual stress value appeared at 20 mm for specimen B, and 25 mm for specimen C. Similar phenomenon was
confirmed in the sectional area after tufftriding and sulphonitriding for residual stress measurement. The phenomenon is
considered to be the result of equilibrium between the residual
stress generated by nitriding and residual stress in the diffusion
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layer 4). Furthermore, hardness distribution curve agreed with

residual stress curve as shown in Figure 8.
As the results showed in the hardness distribution curve,
repeating gas-nitriding under the same condition 7 times
covered a deeper section than when the process is repeated 1
to 3 times. The residual stress distributions curve for depth
prior to the 1.5x104 cycles thermal fatigue test varied greatly
compared to the distribution curve after the test.
Thus, compared to the results prior to the test, the surface
residual compressive stress for each specimen decreased
by approximately -300MPa. This was due to interaction
between decreased residual stress caused by de-nitriding, and
softening from heating. However, comparing the stress affected
depth of the results prior to the test, a slight decrease of
approximately 20 to 30 mm was detected, gradually achieving
the matrix value.
Comparing residual stresses at a depth position of 300 mm,
the residual stress increased slightly from -100 to 180MPa,
compared to -50MPa prior to the test. It was considered that
the reason for this slight increase was due to the thermal stress
produced by repetitive heating-cooling during the thermal
fatigue test.

Measurement of generated crack

Figure 11 shows the measurement of heat-checking(crack)
which developed to matrix after the 1.5x104 cycles thermal
fatigue test. Maximum crack length in both specimens, A and
B was approximately 30 mm, however, the crack length in
specimen C increased notably to 50 mm. Since the maximum
crack length in non-treated specimen, SKD61 is approximately
180 to 190 mm, repeated gas-nitriding specimen produced
a higher heat-checking resistance compared to non-treated
specimens.
In this experiment, specimens were repeatedly nitrided
under the same conditions. Though nitride layer increased
its thickness as nitriding process was repeated, significant
difference was not observed between the initial and second
nitriding process. Maximum crack length in specimen
C was approximately 25 mm larger compared to specimen
A and B. We believe this phenomenon is due to the thicker
nitride layer.
Specimens with thick nitride layer (approximately 10
to 20 mm) and specimens processed with tufftriding and
sulphonitriding showed a crack length as large as 180 to 1100
mm after thermal fatigue test. Increase of nitride layer causes
heat-checking resistance to drop. In the case of specimen
C in this experiment, the thickness of nitride layer was 2
mm, which was substantially lower than the results discussed
earlier. However, it was observed that heat-checking resistance
decreased as nitride layer increased in all specimens.
When nitriding process is repeated while operating the die
and the same result is achieved as in specimen A, heat-checking
resistance will further increase to produce a stable surface.
Analysis of thermal fatigue phenomena in this experiment
showed results of a single process produced under the same
condition. This experiment clarified the relationship between
thermal fatigue characteristics and formation of nitride
layer when repeated peening and gas-nitriding process was
conducted. Thus, a significant fact relative to extending
the life up of die and operating maintenance technique
was established.

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The following are summarized conclusions of the experiment

conducted to study thermal fatigue and residual stress of die
casting die steel surface treated with repeated peening and
gas-nitriding process.
As gas-nitriding process is frequently repeated, the thickness
of nitride layer on the near surface increases which saturated
with excess nitrogen gas.
The surface hardness for specimen B and C increased
approximately 200HV as compared to specimen A, but the
depth of the hardness was the same for all specimens. Increase
in surface hardness was created by development of nitride,
processed repeatedly by gas- nitriding and grain boundary
precipitation of nitride. After the thermal fatigue test, the
surface hardness notably decreased while the hardened depth
area increased.
Measuring the residual stress, specimen A underwent great
compressive stress up to approximately 2x103 cycles. Specimens
B and C showed a low residual stress of approximately 250MPa
less than specimen A. In measuring the surface residual stress
prior to thermal fatigue test, specimen A showed a remarkably
high compressive stress value -1000MPa, while specimens B
and C treated repeatedly with nitriding process showed a
lower stress value -700 to -800MPa.
In the case of specimens B and C, residual stress value after
thermal fatigue test produced a distribution curve indicating
maximum compressive stress value at depth of 20 to 30 mm
from the surface. Residual stress distribution curve after thermal
fatigue test showed a notable decrease in residual stress value,
and a slight increase in the matrix.
The disposition trend of the hardness and residual stress
distribution curves were in agreement for both the surface and
sectional area. These values proved to be effective in evaluating
the die surface by selecting the measuring method.
Evaluating thermal fatigue characteristics of specimens
processed repeatedly with gas-nitriding was considered to be
great value in extending the life up of die and managing the
operation. The issue for future study is to alter the conditions
for gas-nitriding to achieve the same hardness and residual
stress distribution curve.

Table 1 Conditions of X-ray stress measurement.

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