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Materials Science and Engineering A 392 (2005) 348–358

Cavitation erosion resistance of AISI 316L stainless steel laser


surface-modified with NiTi
K.Y. Chiua , F.T. Chenga,∗ , H.C. Manb
a Department of Applied Physics, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, China
b Department of Industrial and Systems Engineering, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, China

Received 15 June 2004; accepted 25 September 2004

Abstract

The present study is part of a project on the surface modification of AISI 316 stainless steel using various forms of NiTi for enhancing
cavitation erosion resistance. In this study, NiTi powder was preplaced on the AISI 316L substrate and melted with a high-power CW Nd:YAG
laser. With appropriate laser processing parameters, an alloyed layer of a few hundred micrometers thick was formed and fusion bonded to
the substrate without the formation of a brittle interface. EDS analysis showed that the layer contained Fe as the major constituent element
while the XRD patterns of the surface showed an austenitic structure, similar to that of 316 stainless steel. The cavitation erosion resistance of
the modified layer (316-NiTi-Laser) could reach about 29 times that of AISI 316L stainless steel. The improvement could be attributed to a
much higher surface hardness and elasticity as revealed by instrumented nanoindentation tests. Among various types of samples, the cavitation
erosion resistance was ranked in descending order as: NiTi plate > 316-NiTi-Laser > 316-NiTi-TIG > AISI 316L, where 316-NiTi-TIG stands
for samples surfaced with the tungsten inert gas (TIG) process using NiTi wire. Though the laser-surfaced samples and the TIG-surfaced
samples had similar indentation properties, the former exhibited a higher erosion resistance mainly because of a more homogeneous alloyed
layer with much less defects. In both the laser-surfaced and TIG-surfaced samples, the superelastic behavior typical of austenitic NiTi was
only partially retained and the superior cavitation erosion resistance was thus still not fully attained.
© 2004 Elsevier B.V. All rights reserved.

Keywords: Laser surface modification; Cavitation erosion; AISI 316L stainless steel; NiTi; Hardness

1. Introduction the degradation process being known as cavitation erosion


[3]. The intensity of cavitation attack depends on the hy-
Cavitation erosion is a common cause leading to damage drodynamic conditions [4] and the properties of the liq-
of components in hydraulic machinery and liquid-handing uid [5]. On the other hand, owing to the special features
systems [1]. In fact, repairing of propellers due to cavita- of cavitation attack, the cavitation erosion resistance of a
tion erosion is a routine service in dockyards. Cavitation, material is a unique mechanical property not directly cor-
which is defined as the generation and collapse of bub- related to bulk properties [6]. Cavitation damage may be re-
bles in a liquid [2], arises from local pressure fluctuation duced by modifying the hydrodynamic conditions to which
within a liquid due to flow or vibration. When bubbles a surface is exposed, and by proper material selection. With
collapse near a solid surface, intense stress pulses are ex- regards to the latter, the design engineer has to make com-
erted on the surface. Repetition of the stress pulses leads promise among different properties and considerations, in-
to plastic deformation, fatigue, and eventually material loss, cluding bulk mechanical properties, corrosion and erosion
properties, fabrication and processing properties, cost, etc.
∗ Corresponding author. Tel.: +852 2766 5691; fax: +852 2333 7629. In this connection, surface modification offers a flexible
E-mail address: apaftche@polyu.edu.hk (F.T. Cheng). and economical route to combat cavitation attack since it

0921-5093/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2004.09.035
K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358 349

can enhance surface properties without altering bulk proper- Table 2


ties. Laser processing parameters and sample designation
AISI 316 stainless steel is a widely used engineering ma- Laser processing parameters
terial in liquid-handling systems and in hydraulic machinery Sample Power (W) Spot size Scanning speed Energy density
by virtue of its excellent corrosion resistance, good proces- (mm) (mm/s) (J/mm2 )
sibility, and relatively low cost. However, its cavitation ero- 316-NiTi-1 700 3 45 5.19
sion resistance is relatively low [7], and this limits its use in 316-NiTi-2 900 3 55 5.45
intensely cavitating environments. To extend its range of ap- 316-NiTi-3 500 3 25 6.67
plications, a feasible way is to employ surface modification 316-NiTi-4 700 3 35 6.67
316-NiTi-5 900 3 45 6.67
at locations which are prone to cavitating attack. In this re-
gards, laser surface modification of 316 stainless steel using
different added materials has been attempted by the present
authors [8–10].
It has been reported that NiTi possesses very high cav- in an Ar atmosphere at 750 ◦ C for 3 h to remove moisture
itation erosion resistance, mainly due to its superelasticity and H2 that were commonly present in NiTi powder. The
[11–14]. In addition, NiTi is comparable to stainless steels in treated powder was then mixed with a binder (4% polyvinyl
corrosion resistance [15] and does not become radioactivated alcohol, PVA) to form a paste and preplaced on the sample
like Co. However, using NiTi in bulk for components might surface by painting to form a layer of 0.4 mm. The samples
not be feasible because of its high cost and poor machinabil- were irradiated with a high-power CW Nd:YAG laser to melt
ity [16]. Thus a practical way is to employ NiTi in surface the NiTi powder under an Ar atmosphere using various pro-
modification, as reported in a number of studies using ex- cessing parameters as shown in Table 2 together with the
plosive welding [17], infrared brazing [13], plasma spraying sample designations (316-NiTi-X). Successive melt tracks
[18], and plasma ion plating [19] on steels, and laser-plasma were overlapped by 50% to form a laser-treated surface. For
hybrid spraying on Ti [20], each with its own merits and comparison, NiTi (austenitic) plates and 316 stainless steel
limitations [21]. Recently, cladding of NiTi wires onto steels samples surfaced with the tungsten inert gas (TIG) process
using the tungsten inert gas (TIG) process for improving cav- using NiTi filler wire [21] (designated as 316-NiTi-TIG) were
itation erosion resistance has been reported [21,22]. The de- also included in the present study.
gree of improvement using the TIG process (by a factor of
9 based on mean erosion rates, and a factor of 3.3 based on 2.2. Metallographic and microstructural analysis
steady erosion rates) was limited by the quality of the clad
layer [21]. The layer contained pores, which are defects com- After laser surface modification, the samples were pol-
monly found in TIG weld surfacing. The present study is an ished with SiC paper and then 1 ␮m diamond paste for cavita-
attempt to employ NiTi powder in the laser surface modifi- tion erosion test. Cross-sections of the samples were similarly
cation of AISI 316L stainless steel. It is part of a project on prepared for microstructural studies, with the polished sur-
the surface modification of 316 stainless steel using various face etched with an acidic etchant (1 part HF, 2 parts HNO3 , 3
forms of NiTi for enhancing cavitation erosion resistance. parts H2 O). The thickness of the laser-modified layer was de-
termined using optical microscopy (Nikon Microphot FXA).
The microstructure was studied using scanning electron mi-
2. Experimental details croscopy (SEM, JEOL JSM-6335F) and the composition was
acquired using energy-dispersive spectroscopy (EDS, JEOL
2.1. Materials and sample preparation EX-64125JMU). The phases present were studied by X-ray
diffractometry (XRD, Philips PW3710) using Cu K␣ gener-
Rectangular samples of thickness 5 mm were spark cut ated at 40 kV and 35 mA.
from AISI 316L stainless steel bars (nominal composition
given in Table 1) of cross-section 12 mm × 20 mm. The sam- 2.3. Indentation tests
ples were sandblasted before powder preplacement to en-
hance adhesion. NiTi powder (nominal composition given The Knoop microhardness at the surface of the samples
in Table 1) of average particle size ∼10 ␮m was degassed and across the cross-section of the samples was measured at
a load of 200 g and a loading time of 15 s (Buehler Micromet
Table 1 II). To study the interfacial toughness qualitatively, two sim-
Nominal composition in wt.% of AISI 316L substrate and NiTi powder ple tests were performed: (a) Vickers indentations were made
Nominal composition in wt.% at the surface layer/substrate interface; (b) the layer was
ground to almost the interface and a heavy load of 330 kg was
Fe Cr Ni Mo Mn Si P S C Ti
applied to a rod 1 mm in radius pressed against the surface.
AISI 316L Bal. 17 12 2.5 2 1 0.045 0.03 0.03 – The nanoindentation properties of the sample surface were
NiTi powder – – 55 – – – – – – 45
probed by a nanoindentation tester (NANO INDENTER II)
350 K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358

with a Berkovich indenter, the maximum load being 200 mN and the weight loss was converted to a mean depth of erosion
and the loading time being 10 s. (MDE) according to:

10W
2.4. Cavitation erosion tests MDE (µm) = (1)
ρA
Cavitation erosion tests were performed using an ultra-
sonic vibratory facility (Misonix XL-2020 Sonicator) con- where W is the weight loss in mg, A is the eroded area in
forming to ASTM Standard G32–92 [23], with the samples cm2 and ρ is the density of the surface layer in g cm−3 . The
in the unattachment mode. The peak-to-peak amplitude and cavitation erosion test was continued for a sufficiently long
the vibration frequency used were 100 ␮m and 20 kHz, re- period until a steady erosion rate was reached. The cavitation
spectively, with a separation of 0.5 mm between the sample erosion resistance Re is defined as:
and the horn tip. The cavitating liquid was deionized water
kept at 23 ◦ C. The sample was weighed at regular intervals Re (h/µm) = (SER)−1 (2)

Fig. 1. Optical micrographs showing (a) cross-section and (b) surface of sample 316-NiTi-4.
K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358 351

Fig. 2. Composition profile along the depth of the cross-section of the alloyed layer in 316-NiTi-4.

where SER is the steady erosion rate in units of ␮m/h. Owing fluence should be larger than 5.4 J/mm2 . When the fluence
to difference in cavitation erosion behaviors among different was too low (samples like 316-NiTi-1), adhesion of the sur-
types of samples, the erosion test time to reach steady erosion face layer and the substrate was poor and the surface layer
varied. became detached from the substrate upon subsequent ma-
The cavitated sample surface at the end of the test was chining. The other laser-treated samples were subjected to
studied by SEM. cavitation erosion tests (results reported in 3.3) and the most
resistant sample, 316-NiTi-4, was selected for detailed com-
3. Results and discussion positional, microstructural, and indentation studies.
The optical micrographs in Fig. 1(a) and Fig. 1(b) show
3.1. Composition and microstructure of laser-treated the cross-section and the surface of 316-NiTi-4, respectively.
layer A modified layer of a few hundred ␮m without cracks or
pores was formed, as shown in Fig. 1. On the other hand, it
Results of preliminary trials on the laser processing param- was noted that pores were common in 316-NiTi samples sur-
eters suggested that for satisfactory layer quality, the laser faced with the TIG process using filler wires. The pores were

Fig. 3. XRD patterns for AISI 316L, NiTi powder, and 316-NiTi-4.
352 K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358

The elements were uniformly distributed in the layer, with a


narrow transitional region of about 50 ␮m thick. Fe was the
major constituent in the modified layer. The XRD patterns in
Fig. 3 reveals that the alloyed layer in 316-NiTi-4 had a struc-
ture similar to that of AISI 316L (i.e., ␥-Fe) rather than the
B2 structure of NiTi powder, consistent with the EDS results.
The SEM micrographs in Fig. 4 show the microstructure
of the alloyed layer near the surface, at the middle, and at the
layer/substrate interface. The microstructure was fairly ho-
mogeneous in these regions. The grain size was of the order
of a few ␮m, with the grain size becoming smaller near the in-
terface, possibly due to a higher cooling rate there. Compared
with the TIG-surfaced samples [21], the laser-treated sam-
ples had a more homogeneous microstructure. Small pores
that were present in the TIG-surfaced samples were absent
in the laser-alloyed layer.

3.2. Indentation properties

The Knoop microhardness on the alloyed surface and


along the depth of the cross-section of the alloyed layer
(Fig. 5) was around 700 HK, which was comparable to that
of the 316-NiTi-TIG samples [21] and much higher than that
of AISI 316L (180 HK) and austenitic NiTi (∼400 HK). In
fusion bonding Ti alloys to steels there has been concern on
the embrittlement of the interface due to the formation of
brittle intermetallic phases [25,26]. The brittleness or frac-
ture toughness may be quantitatively or qualitatively stud-
ied by indentation tests [27,28] by observing the formation
of cracks at the indentation. No cracks were observed in the
Vickers indentation at the interface of the laser-treated sample
316-NiTi-4 (Fig. 6). Heavy deformation of the laser-treated
sample near the interface (the top portion of the surface layer
had been deliberately removed) also did not show any crack-
ing (Fig. 7). The results of these two simple tests, together
with the indirect evidence that the samples were capable of
withstanding rough handling like cutting and grinding, indi-
cated that the interface and the layer were tough. This could
be attributed to a high Ni content [29] and the absence of a
continuous brittle intermetallic phase [30].
The load-displacement curves acquired in nanoindenta-
tion tests for AISI 316L, NiTi plates, laser-surfaced and TIG-
surfaced samples are shown in Fig. 8. Unlike conventional
indentation tests which rely on the indent after unloading
and provide information on plastic deformation only, instru-
mented nanoindentation tests probe both elastic and plas-
Fig. 4. SEM micrographs showing the microstructure of the cross-section
of the alloyed layer in 316-NiTi-4 (a) near the top, (b) in the middle, and (c) tic properties [31]. The nanoindentation characteristics of
near the layer/substrate interface. the laser-surfaced and the TIG-surfaced samples were quite
similar. The surfaced samples were much harder than AISI
possibly formed by the presence of gasses originating from 316L as evidenced by a much smaller maximum displace-
various sources [21,24]. The better quality of the laser-treated ment (dmax ) reached. In addition, they were more elastic than
samples could be attributed to the laser process, which is a 316L as indicated by the elastic recovery ratio r (defined as the
more refined and controllable process than the TIG process, fraction of maximum displacement recovered upon unload-
and to the use of baked NiTi powder. ing). Compared with NiTi plate, the value of the elastic re-
Fig. 2 shows the composition profile along the depth of a covery ratio for the surface treated samples was substantially
typical modified layer (316-NiTi-4) as determined by EDS. reduced (from 39% to 28–29%), indicating that the supere-
K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358 353

Fig. 5. Hardness profile along the depth of the cross-section of the laser-modified layer.

lasticity of NiTi was only partially retained, but accompanied with different processing parameters owing to difference in
by an increase in hardness. the quality of the surface layer. Sample 316-NiTi-4 was the
least defective one and the degree of erosion was the least.
3.3. Cavitation erosion behavior
This was the sample that had been chosen for detailed com-
Curves for the mean depth of erosion (MDE) as a function positional and microstructural studies, and for comparison
of time are shown in Fig. 9 for various laser-treated samples. It with the TIG-surfaced sample and NiTi plate. In the other
can be observed that the erosion rate was much reduced after laser-treated samples, cracks and pores were present, as re-
laser treatment. The MDE varied among the samples treated vealed by the SEM micrographs in Fig. 10. The presence and

Fig. 6. Vickers indentation at the interface.


354 K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358

Fig. 7. Optical micrograph showing the interfacial region after heavy deformation.

Fig. 8. Force-displacement curves in nanoindentation test. r is the elastic recovery ratio defined as the fraction of maximum displacement recovered upon
unloading.

Fig. 9. Mean depth of erosion (MDE) as a function of time for laser-treated samples in cavitation erosion test in deionized water.
K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358 355

the severity of defects in these samples were reflected in the Fig. 11(a) shows the erosion curves for AISI 316, 316-
relative ranking of the cavitation erosion resistance depicted NiTi-4, 316-NiTi-TIG, and NiTi plate. These samples exhib-
in Fig. 9. ited large difference in cavitation erosion behavior and in the
erosion test time required to obtain the steady erosion rate.
For example, the time required for AISI 316L was only 6 h,
but that for NiTi plate, 30 h. In view of this, the cavitation
erosion resistance Re was calculated from the steady erosion
rate (SER) instead of the mean erosion rate (MER), which
is affected by the test time. For easy comparison, the cavita-
tion erosion resistance is normalized (denoted as Rne ) relative
to AISI 316L (Rne = 1) and shown in Fig. 11(b). The prop-
erties and erosion resistance of various types of samples are
summarized in Table 3.
Laser surface modification of AISI 316L with NiTi re-
sulted in a large increase in the cavitation erosion resistance,
which could reach about 29 times by the method employed
in the present study. It is obvious that both high hardness and
high elasticity would contribute to high cavitation erosion re-
sistance. Thus the large increase in erosion resistance after
laser treatment could be attributed to a modified layer which
was much harder (700 HK for 316-NiTi-4 versus 180 HK for
substrate) and more elastic as reflected by a higher elastic
recovery ratio in the nanoindentation tests. It is interesting to
note that although the TIG-surfaced sample possessed similar
indentation properties (in terms of hardness and elastic recov-
ery ratio) as the laser-surfaced one, the erosion resistance of
the former was lower mainly because it contained more de-
fects, which acted as sites for initiation and propagation of
erosion damage. On the other hand, the erosion resistance of
the laser-surfaced samples was inferior to that of NiTi plates,
though the hardness was higher. Austenitic NiTi possesses a
very high cavitation erosion resistance, mainly by virtue of
its superelasticity which allows it to receive intense cavita-
tion pulses with minimal damage [13,32]. The nanoindenta-
tion test results showed that superelasticity was only partially
retained in the laser-treated samples and thus the superior
cavitation erosion resistance of NiTi was not fully attained.
This suggests that superelasticity is more contributive to high
cavitation erosion resistance than hardness. In summary, the
difference in cavitation erosion resistance for different types
of samples (316L, 316L modified with NiTi, and NiTi plate)
could be attributed to the difference in indentation proper-
ties (elasticity and hardness), with elasticity playing a more
important role. For samples of the same type (laser-surfaced
and TIG-surfaced 316 samples), the difference in resistance
could be attributed to the quality of the surface layer. Thus
improved processing techniques/conditions that can deposit
an intact NiTi layer minimally diluted by the substrate would
be expected to result in a higher erosion resistance than that in
the present study, and attempts in this direction are underway.
Apart from a large increase in the erosion resistance by
laser surface modification, the mode of material removal
from the surface also changed. Fig. 12 shows the surface
appearance of AISI 316L and the laser-surface sample 316-
Fig. 10. SEM micrographs showing defects (cracks and pores) in some laser- NiTi-4 after the cavitation erosion test. AISI 316L exhibited
treated samples: (a) 316-NiTi-2, (b) 316-NiTi-5, and (c) 316-NiTi-3. an eroded surface typical of ductile rupture, consistent with
356 K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358

Fig. 11. Comparison of cavitation erosion behaviors of AISI 316L, 316-NiTi-4, NiTi plate and 316-NiTi-TIG: (a) erosion curves, and (b) normalized cavitation
erosion resistance Rne .

its low hardness. On the other hand, 316-NiTi-4 exhibited This is consistent with the partial superelasticity present in
a damaged surface with cracks of erosion (test time: 12 h, the laser-surfaced samples. Similar surface appearance for
Fig. 12(b)) similar to that of NiTi tested to a much longer NiTi in cavitation erosion test was also reported by others
time (test time: 40 h, at a higher magnification, Fig. 12(c)). using the attachment mode of test [33].

Table 3
Properties and cavitation erosion resistance of various types of samples
Surface Knoop Nanoindentation, maximum load = 200 mN Cavitation erosion Normalized cavitation
hardness (HK) resistance, Re (h/␮m) erosion resistance, Rne
Maximum deformation, dmax (nm) Elastic recovery ratio, r (%)
AISI 316L 180 1659 8.4 0.26 1
316-NiTi-TIG 700 1045 29.6 0.86 3.3
316-NiTi-4 728 1061 28.1 7.49 28.8
NiTi plate 400 1344 39.4 11.55 44.4
K.Y. Chiu et al. / Materials Science and Engineering A 392 (2005) 348–358 357

ties and the cavitation erosion behavior of the laser-surfaced


samples have been studied. The following conclusions are
drawn.With proper laser processing parameters, a NiTi-
modified layer of a few hundred ␮m thick was formed on AISI
316L substrate. The layer was free of cracks and pores and
bonded strongly to the substrate with a tough interface.The
microstructure of the modified layer was homogenous and
fine-grained, with grain size of a few ␮m.Compared with
the substrate, the modified layer had a much higher micro-
hardness (700 HK versus 180 HK), and a higher elastic re-
covery ratio in nanoindentation test (28% versus 8%). A
large increase in the cavitation erosion resistance, reaching
about 29 folds, was achieved, the increase being attributable
to improved indentation properties.Laser surface processing
brought about a larger increase in cavitation erosion resis-
tance than the TIG process reported in a previous study be-
cause of the formation of a more uniform and less defective
alloyed layer.

Acknowledgements

The work described in this paper was fully supported by


a grant from the Research Grants Council of the Hong Kong
Special Administrative Region, China (Project No. PolyU
5252/03E). Support from the infrastructure of the Hong Kong
Polytechnic University is also acknowledged.

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