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Nitriding Ingles
Nitriding Ingles
Original Article
Article history: In this work, the effect of the nitriding process on microstructure and mechanical prop-
Received 16 April 2022 erties of additively manufactured (AM) 17-4PH stainless steel is investigated. The nitriding
Accepted 31 May 2022 was performed at 530 C, 560 C, and 580 C for 2 h. The nitriding process improves the
Available online 11 June 2022 hardness and surface roughness of the AM 17-4PH steel. Detailed microstructural char-
acterizations of both as-built and nitride samples are performed using an optical micro-
Keywords: scope, scanning electron microscope (SEM) equipped with energy-dispersive X-ray
17-4PH steel spectroscopy (EDS), and X-ray diffraction technique. It reveals that the nitride layer
Nitriding thickness increases with nitriding temperature. A distinct transition layer between the
Micro-hardness substrate and nitride layer is observed in the 560 C and 580 C nitride samples. The
Surface roughness nitriding process develops almost equiaxed grain microstructure with new secondary
Precipitates phase precipitates, whereas in the as-built material, the grains are primarily columnar
DMLS along the AM process build direction. Specifically, the nitriding process introduces g-Fe4N,
ε-Fe3N, CrN, and Ni3N precipitates. The increase in Ni- and Cu-rich precipitates with the
nitriding temperature explains the observed improvement in the hardness and surface
roughness. Furthermore, the nitriding process does not alter the substrate's initial weak
crystallographic texture.
© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
* Corresponding author.
E-mail addresses: rajiniklu@gmail.com, n.rajini@klu.ac.in (N. Rajini).
https://doi.org/10.1016/j.jmrt.2022.05.198
2238-7854/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 1 9 : 2 8 1 0 e2 8 2 1 2811
Fig. 1 e The effect of nitriding temperature on the layered structure: SEM micrographs of samples nitrided at (a) 530 C, (b)
560 C, and (c) 580 C; and (d) the corresponding EDS line mapping of nitrogen for all three temperatures. The nitriding
process develops the nitride layer and adjacent transition layer. The latter is not visible for the case of nitriding at 530 C.
Here NL, TL, and SS stand for nitride layer, transition layer, and substrate, respectively. (e) Average nitride layer thickness as
a function of the nitriding temperature. The error bar represents the variation in the layer thickness.
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Fig. 2 e Micro-hardness profiles of 17-4PH steel from the sample surface into the substrate for different nitriding
temperatures. Hardness tests were performed with a spacing of 10 mm using a diamond indenter (figure inset). The vertical
dashed lines represent the measured nitride layer thickness.
2814 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 1 9 : 2 8 1 0 e2 8 2 1
measured top-surface microhardness values of 17-4PH steel 3.3. Effect of nitriding process on surface roughness
and the values from the literature. First, the as-built DMLS 17-
4PH steel exhibits better microhardness than the sintered/ Figure 3 shows the surface roughness of the as-built and
wrought material. The nitriding process improves the surface nitrided samples measured using the surface profilometer.
hardness significantly compared to the as-built material. The measurement was repeated five times, and the observed
Similar observations have also been reported for wrought 17- variation was represented via error bars in Fig. 3. The nitriding
4PH steels [43,57]. Further, an increase in the nitriding process decreases the surface roughness compared to the as-
Fig. 4 e Backscattered microscopy images of the top surface of (a) As-built (AB) and nitrided at (b) 530 C, (c) 560 C, and (d)
580 C 17-4PH steel samples.
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Fig. 6 e Optical images of (a) as-built and (c) 530 C nitrided samples cross-section. (b), (d) and (e) show the enlarged view of
the grain morphology before and after nitriding. For the nitrided sample, the image was taken near the transition layer to
understand the effect of nitriding on the substrate material.
2816 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 1 9 : 2 8 1 0 e2 8 2 1
Fig. 7 e XRD analysis of the as-built and nitrided 17-4PH steels for various temperatures. The measurement was performed
on the top surface of the sample.
the presence of both inter and intra-granular precipitates [59]. similar observation has been reported elsewhere [22,26]. On
To identify these precipitates, a detailed characterization the other hand, the nitriding process develops new phases
using X-ray diffraction and SEM-EDS is performed and pre- and evolves with nitriding temperature. At 530 C, we don't see
sented in Sections 3.5 and 3.6. distinguishable peaks for either the parent martensite or new
To understand the effect of the nitriding process on the phases. The observed overlapped peaks look similar to the
substrate, the microstructure was studied near the transition ‘amorphous-like’ features, which might lead to the bright
layer (just below the nitride layer). For comparison purposes, contrast seen in the microscopy image shown in Fig. 4(b).
the microscopic image of the as-built sample cross-section is Later, we see a clear transition from the non-crystalline
shown in Fig. 6(a). The magnified view in Fig. 6(b) shows the (amorphous-like) to crystalline pattern with an increase in
AM process developed columnar microstructure. Mostly, the the nitriding temperature [60]. At 560 C, we see clear and
long axes of the columnar grains are parallel to the build di- distinguishable peaks of a-Fe, CrN, Fe3N, Fe4N, and a0 N
rection. Similar to the top surface shown in Fig. 4(a), the pre- compared to 530 C. However, the observed peaks are broad-
cipitates are randomly distributed along the grain boundaries ened. It may be due to the formation of the a0 N (expanded
and within the grains. Cross-sectional optical image of the austenite) phase during the nitriding process and the possi-
530 C nitrided sample is shown in Fig. 6(c), and the magnified bilities of local defects around the a0 N phase. The presence of
view of the region near the transition layer is shown in Fig. 6(d) the a0 N phase distorts the lattice locally and thus develops
and (e). high internal residual stresses, which broadens the diffraction
Unlike the as-built material, the grains are almost equi- peaks [61,62]. At 580 C, CrN and a-Fe peaks intensify, and at
axed with a lath structure. Also, the size of the grains in the the same time, a0 N disappears. This is due to the formation of
nitrided samples is smaller than in the as-built sample, as CrN precipitates by depleting the Cr from a0 N (a0 N / a þ CrN)
seen in Fig. 6(e). The reduction in grain size is potentially due [51]. The other observed peaks at 580 C were g-Fe4N, ε-Fe3N,
to the formation of intragranular precipitates and partial and Ni3N.
recrystallization. Similar observations were reported by Van-
der Voot et al. by comparing the microstructures of untreated 3.6. Characterization of precipitates
and H1100 solution heat-treated 17-4PH steels [55].
In this section, the types and morphology of the precipitates
3.5. Phase analysis of the nitride layer are studied using backscattered SEM imaging and EDS. The
left column of Fig. 8 shows the top surface SEM images of the
X-ray diffraction (XRD) analysis was conducted to identify the samples that are nitrided at (a) 530 C, (c) 560 C, and (e) 580 C.
phases for the as-built and nitrided samples. XRD diffracto- The inset in Fig. 8(b), (d) and (f) represents the mean weight
gram of as-built and all three nitrided 17-4PH samples are percentage and standard deviation of the elements present in
shown in Fig. 7. The diffraction was performed on the top each spectrum. Based on the shape and color contrast, we
surface of the nitrided samples. XRD diffractograms of the as- observe three different precipitates: rod-like bright features,
built sample reveal that it is mainly dominated by the a-Fe black and greyish spherical precipitates. All these three types
phase with a smaller amount of g-Fe (austenite phase). A of precipitates are present in all the nitriding cases. A detailed
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Fig. 8 e Backscattered electron microscopy image of nitrided 17-4PH steel at 530 C (a), 560 C (c), and 580 C (e) with EDS
results showing the presence of (b) nickel-rich precipitates (d) copper-rich precipitates and (f) niobium-rich precipitates.
Figure inset on (b), (d) and (f) indicates the mean weight and standard deviation of all elements present in each spectrum.
EDS analysis reveals that the bright rod-like precipitates are during corrosion attacks [1,64]. Compared to Ni-rich pre-
rich in Ni, whereas the black and greyish precipitates are rich cipitates, the Cu-rich precipitates are smaller and uniformly
in Cu and Nb, respectively. Experimentally acquired EDS distributed in the microstructure. Interestingly, the presence
spectrum for a few precipitates are shown in the second row of Cu-rich precipitates increases with the nitriding tempera-
of Fig. 8. Spectrum analysis of Ni- (spectrum 7 and 9), Cu- ture. A similar observation has been reported in [1], wherein
(spectrum 37 and 38) and Nb- (spectrum 50 and 54) rich pre- Cu-rich precipitates are formed only after solution heat
cipitates are shown in Fig. 8(c), (e) and (g), respectively. treatment at 1040 C and subsequent aging at 472 C for 1hr.
The Ni-rich precipitates are commonly observed in 17-4PH The initial solution heat treatment at 1040 C does not form
steels [63], and thus increase the high-temperature mechan- Cu-rich precipitates in the samples. Similarly, Jiang et al. also
ical strength [14]. The presence of Ni-rich precipitates also showed that the Cu-rich precipitates are spherical, and their
promotes the stability of the protective oxide film and reduces density increases with heat treatment temperature [65].
both pitting and crevice corrosion propagation that occurs Extensive literature suggests that the increase in Cu-rich
2818 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 1 9 : 2 8 1 0 e2 8 2 1
Fig. 9 e Stereographic pole figures as measured using X-ray diffraction technique in the (a) as-built and (b) 580 C nitrided
17-4PH steel.
precipitates increases the hardness and yield strength of the grain growth during the AM process. Similar observation, i.e.,
material. [66e68] This explains the observed increase in the random crystallographic orientation, has been reported for
microhardness with nitriding temperature; see Fig. 2 and 17-4PH steel fabricated using DMLS [25], selective laser
Table 2. Nb-rich precipitates are primarily observed in the melting [72], Laser Direct Metal Deposition [73], and Wire Arc
580 C nitrided sample. Commonly, Nb-rich precipitates are Additive manufacturing processes [74]. After the 580 C
formed along the grain boundaries of 17-4PH steel [69], and nitriding process, the material exhibits weak texture, see
thus, it reduces the solid-solution strengthening [70]. In the Fig. 9(b), similar to that in the as-built sample. Thus, it sug-
present study, the amount of Nb-rich precipitates is less than gests that the nitriding process does not alter the crystallo-
other precipitates, hence not affecting the hardness signifi- graphic texture noticeably, while it improves the surface
cantly. At the same time, Nb-rich precipitates are known to properties.
improve the surface roughness via grain refinement [71]. This
also explains the observed improvement in the surface
roughness with the nitriding temperature, see Fig. 3. Overall, 4. Summary
this detailed characterization of precipitates suggests that the
hardness and surface roughness of the materials can be In this work, the effect of the nitriding process on additively
modulated by controlling the precipitate types and their size. manufactured 17-4PH steel is investigated at three different
nitriding temperatures (530 C, 560 C, and 580 C) for a fixed
3.7. Influence of nitriding on crystallographic texture duration of 2 h. The nitriding process increases the surface
hardness approximately three times compared to the as-built
In this section, the effect of the nitriding process on the condition. The surface roughness is reduced significantly by
crystallographic texture is investigated. Incomplete pole fig- the nitriding process, and most importantly, it decreases more
ures of the samples are obtained using the X-ray diffraction with an increase in the nitriding temperature. Detailed
technique. Figure 9 shows the (110) (200), and (211) pole figures microstructural characterization reveals that the nitriding
taken on a plane parallel to the rod axis, i.e., build direction for process (i) changes the columnar grain structure to more of an
the (a) as-built and (b) 580 C nitrided samples. equiaxed; (ii) develops different types of inter and intra-
There is no preferred orientation in the as-built sample, granular precipitates; (iii) does not alter the initial weak
which may be a consequence of static recrystallization and crystallographic texture. These microstructural observations
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 1 9 : 2 8 1 0 e2 8 2 1 2819
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Declaration of Competing Interest
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