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Cavitation erosion behaviour of niobium
S.F. Brunatto
a,
, A.N. Allenstein
b
, C.L.M. Allenstein
c
, A.J.A. Buschinelli
d
a
Departamento de Engenharia Mecnica, Universidade Federal do Paran (UFPR), 81531-990, Curitiba, Paran, Brazil
b
Programa de Ps-Graduac o emEngenharia e Cincia dos Materiais, Universidade Federal do Paran (UFPR), 81531-990, Curitiba, Paran, Brazil
c
Departamento Acadmico de Mecnica, Universidade Tecnolgica Federal do Paran (UTFPR), 80230-901, Curitiba, Paran, Brazil
d
Departamento de Engenharia Mecnica, Universidade Federal de Santa Catarina (UFSC), 88040-900, Florianpolis, Santa Catarina, Brazil
a r t i c l e i n f o
Article history:
Received 24 December 2010
Received in revised form26 August 2011
Accepted 6 September 2011
Available online 12 September 2011
Keywords:
Cavitation erosion
Niobium
CA-6NMmartensitic stainless steel
Fatigue
Power generation
a b s t r a c t
Cavitation erosion behaviour of niobium was investigated by means of a 20kHz ultrasonic vibrator at
peak-to-peak amplitude of 50 m, aiming to determine the niobium potential as a material for the man-
ufacturing of hydraulic machine components. The study was emphasized for the three rst cavitation
stages of the cumulative erosiontime curve. The modication of the niobium surface morphology as a
function of the testing time in the incubation, acceleration, and maximum erosion rate stages was veri-
ed by SEM analysis. Samples were prepared from 98.9% purity and 90% reduction cold-rolled niobium
bar. The study was performed for niobium samples in both the cold-worked and annealed conditions.
Samples of CA-6NM martensitic stainless steel, a typical material utilized for hydraulic turbines man-
ufacturing, were also analysed for comparison purpose. Annealing treatment of niobium decreases its
hardness and increases its ductility, leading to an increase of the incubation period when compared with
thecold-worked niobium. Cavitation erosion failure mechanism in niobium occurs in a sequence of events
comprising the work-hardening effect and the fracture of debris allied to the effect of fatigue and micro-
cracks formation. Finally, annealed niobium presents similar incubation period but worse behaviour in
the maximum erosion rate stage than CA-6NM steel.
2011 Elsevier B.V. All rights reserved.
1. Introduction
Cavitation erosion of metals is characterized by local impacts of
uid against the metallic surface due to collapse of bubbles, result-
ing in progressive loss of original material from the solid surface,
in the vicinity of the active cloud within a liquid. Some problems
related to cavitation are vibration in hydraulic machines, increase
in hydrodynamic drag and change in hydrodynamic ow, noise,
thermal and light effects like luminescence, besides erosion wear
[1]. Erosion wear has demanded special attention of researchers
and engineers mainly in power generation plants. This is due to the
high costs associated to preventive and corrective maintenance of
hydraulic machine components, which are continually exposed to
cavitation.
Rayleigh was the rst to study the phenomenon of cavitation
erosion in ship propellers, in 1917 [2]. Afterwards many works
have been performed in this eld, comprising the study of differ-
ent materials, cavitation erosion testing, failure mechanisms and
applications.

Corresponding author. Tel.: +55 41 3361 3231; fax: +55 41 3361 3129.
E-mail address: brunatto@ufpr.br (S.F. Brunatto).
The relative resistance of materials to cavitation erosion is com-
monly determined by mass loss measurements in laboratory, using
ultrasonic vibratory apparatus. The cavitation erosion resistance
has been reported in terms of two quantities, the nominal incu-
bation period (IP) and the maximum or steady state erosion rate
(MER).
Fig. 1 shows typical cavitation stages in cumulative erosion
(material mass loss)time curve. In this case, the erosion has been
characterized by the cumulative mass loss (CML), and the nominal
IP as the initial stage of the erosion ratetime pattern during which
the erosion rate is zero or negligible compared with later stages,
in accordance with ASTM G32-09 [3]. In addition, the maximum
erosion rate (MER) has been dened as the maximum instanta-
neous erosion rate in a test that exhibits such a maximumfollowed
by decreasing erosion rates, and the average erosion rate (AER) as
the cumulative erosion divided by the corresponding cumulative
exposure duration, an amount expressed in mg/h unit [3].
The cavitation erosion resistance of several high purity metals
(Al, Co, Cr, Cu, Fe, Mg, Mo, Ni, Wand Zi) and alloys (copper-, iron-,
nickel- and cobalt-base alloys) was investigated in [5]. It was veri-
ed that the cavitation erosion resistance of the studied materials
is determined by the binding energy, the crystal structure of the
base metal, and the ability of alloys to deformand to achieve phase
transformation.
0043-1648/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2011.09.001
S.F. Brunatto et al. / Wear 274275 (2012) 220228 221
Fig. 1. Typical cavitationstages inthe cumulative erosion(material mass loss)time
curve.
Adapted fromChiu [4] and ASTMG32-09 [3].
An overview of cavitation erosion indicates that four differ-
ent categories of materials has been studied: (a) ferrous alloys,
comprising pure iron, cast iron, and steels [420]; (b) non-
ferrous metals and alloys, such as Al, Cu, Ni, Ti, brass, bronze
[46,12,18,2033]; (c) ceramics and intermetallics [3438]; and
(d) surface treated alloys [17,23,3849]. Up till now, niobiumsub-
strates have not been considered for studies of cavitation erosion.
Niobiumis a refractory and ductile metal. It does not tarnish or
oxidize at roomtemperature. Its mechanical properties are highly
dependent of the content of interstitial elements. Table 1 summa-
rizesomecharacteristics of highpurityniobium, inaccordancewith
[50].
In melting, contaminants such as oxygen, nitrogen, carbon and
hydrogen must be excluded, as soon as possible. High-vacuum
techniques purify niobium, in the solid state at temperatures
above 1980

C by means of NbO
2
volatilization [50]. According to
[51], temperatures of 9001200

C are recommended for niobium


recrystallization purpose. The maximum cold-work reduction
between anneals are virtually unlimited [50]. Considering cold-
worked niobium with 70-80% reduction, it is full recrystallized in
1h at 1090

C [50].
In this work, the cavitation erosion behaviour of niobium was
investigated for both the cold-worked and annealed conditions.
Samples of ASTMCA-6NMmartensitic stainless steel wereanalysed
for comparison purpose, considering that it is typical material uti-
lizedinmanufacturing of hydraulic turbines. The niobiumpotential
as a material for the manufacturing of hydraulic machine compo-
nents was determined by studying the three rst cavitation stages
of the cumulative erosiontime curve. Finally, the modication of
the niobium surface morphology as a function of the testing time
in the incubation, acceleration, and maximum erosion rate stages
was also veried.
2. Experimental procedure
Samples of niobiumcut by wire electrical discharge machining
(WEDM) in dimensions of 20mm 35mm5mm were prepared
from98.9% purity and 90% reduction cold-rolled niobiumbars. The
study was performed for niobiumsamples in both the cold-worked
and annealed conditions. Annealing treatment of the cold-worked
niobiumsamples was carried out in vacuumfurnace, at 1000

C, for
60min, and 1.33Pa pressure.
Samples of ASTM CA-6NM martensitic stainless steel (com-
position in weight %: 0.032% C, 12.25% Cr, 4.42% Ni, 0.63% Mn,
0.522% Si, 0.43% Mo and the balance, Fe) cut for dimensions of
20mm30mm10mm were prepared froma melted bar, which
was quenched and tempered for 22 HRC, presenting typical tem-
pered structure, in the case cubic martensite (bcc-, as Table 1).
The microstructure characterization of niobiumwas performed
using the standard metallographic procedures and scanning elec-
tron microscopy (SEM). After cut, niobiumspecimens were ground
using 220, 400, 600, and 1200 SiC sand-paper. Polishing of the sam-
ples was performedintwo stages, using: (a) 1.0mdiamondpaste;
and (b) 0.05m Al
2
O
3
solution. The etchant was 30ml HF +15ml
HNO
3
+30ml HCl solution, which is in accordance with ASTM 66
standard. The grain size characterization of the annealed niobium
samples was determined according to ASTM E-112 standard. The
ASTMgrain-size number was dened by Eq. (1):
n = 2
N1
(1)
where n is the number of grains per square inch as seen in a spec-
imen viewed at a magnication of 100, and N is the ASTM grain
size number.
Characterization of the phases in the studied materials was per-
formed by X-ray diffractometry (XRD), using Shimadzu equipment
and copper tube, for 2 conguration varying from30

to 120

.
Prior to perform the cavitation testing, the surfaces of cold-
workedniobiumsamples were preparedintwodifferent stages: (a)
aiming to remove typical surface damages due to the cold-rolling
process, samples were ground using 220, 320, 400, 600 and 1200
SiC sand-paper and polished using 1.0mdiamond paste; and (b)
aiming to obtain the nal nishing of the testing surfaces, samples
were over again ground and polished in two steps, using 1.0m
diamond paste for the rst step, and 0.05m Al
2
O
3
solution for
the second one. The same procedure was applied to prepare the
surfaces of the ASTMCA-6NMsteel samples.
On the other hand, annealed niobiumsamples were studied for
two different surface conditions:
(a) Condition 1 (C1): cold-worked samples presenting surfaces in
the nal nishing state, which were submitted to the annealing
treatment and then submitted to the cavitation testing; and
(b) Condition 2 (C2): a second set of samples, comprising samples
of the condition C1, which were over again ground and pol-
ished after the annealing treatment, and then submitted to the
cavitation erosion testing.
In order to characterize the surface nishing of the samples
previously to the cavitation erosion testing, measurements of
roughness were performed in accordance with ISO4287 (1997), for
Table 1
Characteristics of annealed niobium presenting 100200ppm of interstitial contaminants, in accordance with [50], and ASTM CA-6NM steel in accordance with ASTM
A743/A743M/95.
Material Crystal structure Elongation (%) Hardness (HV) Tensile strength (MPa) Yield strength (MPa) Elastic modulus (GPa)
Niobium bcc Unlimited 80 275 207 103
CA-6NM bcc- 15 (min) 250 755 (min) 550 (min) 210
222 S.F. Brunatto et al. / Wear 274275 (2012) 220228
both the materials. The Ra and Rz roughness of the tested surface
was also determined as a function of the testing time for annealed
niobiumsamples using Mahr (Concept) equipment, Gauss lter, for
4mmmeasurement length and ve divisions of 0.80mm. In addi-
tion, aiming to determine the effect of the heat treatment on the
niobium characteristics, hardness measurements in Vickers scale
were realized using a Shimadzu HMV-2T apparatus with a load of
1N.
The cavitation experiments were made in a standard vibratory
cavitation erosion tester as a function of testing time, according
to ASTM G 32-09 [3]. Samples were cavitated in ultrasonic vibra-
tory equipment via indirect method. The experimental apparatus
utilized here for cavitation test was the same presented in [52].
The vibratory frequency and the peak-to-peak amplitude were
202kHz and 501.0m, respectively. The tip of the probe was
machined from AISI 304 stainless steel and polished for 1.0m
surface roughness. The temperature of the deionised water bath
was maintained at 211.0

C. The surface of the test specimen was


immersed 10mmin deionised water, distant 0.50.005mm from
the probe tip. The mass loss of the test specimens was determined
by means of 0.1mg precision balance.
Cold-worked niobium samples were submitted to cavitation
erosion testing time of 130min. The mass loss measurements were
obtained for partial times of 10min. Otherwise, annealed niobium
samples were tested up to 240min, and the mass loss measure-
ments were taken for different partial times of 10, 20 and 30min,
as indicated in the results. For comparison purpose ASTM CA-
6NMsteel samples were also prepared and submitted to cavitation
erosion testing. Experiments were repeated to conrm the repro-
ducibility of results.
Finally, tested surfaces were characterized by scanning elec-
tron microscopy (SEM), using Philips XL-30 equipment, aiming to
determine the changes of the surface morphology as a function of
the testing time and the cavitation erosion failure mechanism of
annealed niobium.
3. Results and discussions
(a) Characterization of the studied materials
Fig. 2 shows a schematic representation of the samples geome-
try in relation to the testing surface and the rolling direction. It is
also presented typical results of Ra and Rz roughness of 0.04 and
0.28m, and 0.02 and 0.19m, for niobium (Fig. 2a) and ASTM
Table 2
Vickers microhardness obtained for annealed and cold-worked niobium, and CA-
6NMsteel samples.
Material HV
0.1
average value (standard deviation)
Cold-worked niobium 79 (7)
Annealed niobium 127 (3)
ASTMCA-6NMsteel 248 (5)
CA-6NMsteel (Fig. 2b), respectively, characterizing the start condi-
tions of the samples surface prior to the cavitation testing.
Microstructures of the cold-workedandannealedniobiumsam-
ples are presented in Fig. 3. Results indicate that annealed niobium
samples present full recrystallized microstructure (Fig. 3b), since
there is no evidence of a deformed structure as shown in Fig. 3a.
The characterization of the grain size for annealed niobiumhas evi-
denced an average size of 8m, which is equivalent to ASTMgrain
size number 11.
As shown in Table 2, the microhardness value obtained for
annealed niobiumis in agreement with the expected (see Table 1),
conrming that niobium was fully recrystallized in the annealing
treatment (Fig. 3b). Hardness of 79, 127and248HV
0.1
was obtained
for annealedandcold-workedniobium, andCA-6NMsteel samples,
respectively.
Fig. 4 shows typical X-ray diffraction patterns for samples of
niobium(at the top) and CA-6NMsteel (at the bottom). It was evi-
denced that niobiumpresents the bcc (body centered cubic) phase,
and the steel presents two different structures, in the case the bcc
(cubic martensite or -Fe) and the fcc (face centered cubic, austen-
ite or -Fe) phases. The occurrence of austenite in the considered
steel was expected since it usually presents retained austenite in
amounts up to 10vol.% at the tempered condition.
(b) Cavitation erosion behaviour of annealed and cold-worked
niobium
Fig. 5 presents the cumulative mass loss (CML) as a function
of the cavitation erosion time for cold-worked and annealed nio-
biumsamples. It was evidencedthat cold-workedniobiumpresents
smaller cavitation resistance than annealed niobium. This result
could be related to the high degree of work-hardening of the
cold-worked structures. Inaddition, whereas the incubationperiod
(IP) of the cold-worked niobium was on the order of 40min,
annealed niobium presented an incubation period at least two
times longer, in the case on the order of 90min. The difference
Fig. 2. Schematic representation of the sample and typical roughness proles for samples of: (a) niobium; (b) ASTMCA-6NMsteel.
S.F. Brunatto et al. / Wear 274275 (2012) 220228 223
Fig. 3. Microstructures obtained by SEMfor niobiumin the: (a) cold-worked state; (b) annealed state.
Fig. 4. Typical X-ray diffraction patterns for samples of annealed niobiumand CA-
6NMsteel.
couldbeexplainedconsideringtheassumptionthat theenergypro-
vided by the impacts of microjets [53] and/or spherical collapse of
micro bubbles [5456] on the specimen surface would be spent
in higher proportion to produce work of plastic deformation in
annealed niobium, leading to the known effect of work-hardening
[57]. The work-hardening effect precedes the crack formation pro-
cess. So, due to high density of crystalline defects and high degree
of plastic deformation of the cold-worked niobium, a smaller work
of plastic deformation would result in the opening of newsurfaces,
Fig. 5. Cumulative mass loss as a function of the cavitation erosion time for
cold-worked and annealed niobium samples prepared for two different surface
conditions, C1 and C2.
leading preferentially to crack propagation and the failure of the
surface.
Another aspect to be considered is that the surface deforma-
tion requires a high degree of multiple slipping, being necessary
a high effective shear stress to enable the dislocations to cross
slip. In the earliest stages of cavitation erosion testing, plastic
deformation tends to occur and slip lines can be observed inside
individual grains, which display micro-relief as a consequence of
the cavitation impact waves. The intensity of the plastic deforma-
tion is different for each grain due to its own and their neighbours
lattice spatial orientation. Due to restrictions to deformation (slid-
ing and rotation) imposed by the polycrystalline structure, since
grain boundaries are regions of stress concentration and act as
slip barriers, hindering the movement of dislocations, the mass
removal process becomes easier in such regions. As a general rule,
it has been observed grain boundary damaging starts preferen-
tially at boundaries of grains characterized by intense formation
of slip lines and micro-relief. Consequently, during the incuba-
tion period (IP), the mass removal inside the grains tends to
start at weak pits formed in slip lines, and especially at slip line
intersections. As the grains are much more deformed in the cold-
worked than in the annealed condition, higher density of slip
lines could be expected for cold-worked niobium, which would
facilitate the process of mass loss. The above explanation con-
cludes the poor cavitation resistance veried for the cold-worked
niobium.
Moreover, it is to be explained the large dispersion of the cavita-
tion erosion results, evidenced in the maximumerosion rate stage,
for annealed niobiumsamples in the C1 and C2 studied conditions
(see the dashed area in Fig. 5). Samples in the C1 condition could
present surface contamination by interstitial elements, due to O
2
and N
2
residual partial pressures of the vacuum chamber in the
annealing treatment furnace. This assumption is based in the fact
that oxygen presents high reactivity to the niobium and it would
tend to alter the characteristics of the metal surface, leading to a
modication of the cavitation behaviour. On the other hand, for
samples in the C2 condition, the additional step comprising pos-
terior grinding and polishing of the samples after the annealing
treatment would be responsible by eliminating such undesirable
effect, leading to better cavitation erosion behaviour.
Table3summarizes theresults obtainedtodeterminethecumu-
lative mass loss (CML) and the average erosion rate (AER) as a
functionof thetestingtimefor niobiumsamples inthecold-worked
state and for annealed niobiumsamples in the C2 condition.
The CML of the cold-worked niobiumand annealed niobiumin
the C2 condition was 0.1, 3.5 and 46.2mg, and 0, 0.4 and 1.0mg
for testing time of 10, 50 and 100min, respectively. The AER of the
cold-worked niobium and annealed niobium in the C2 condition
was 0.6, 4.2 and 27.7mg/h, and 0, 0.5 and 0.6mg/h for testing time
of 10, 50 and 100min, respectively.
224 S.F. Brunatto et al. / Wear 274275 (2012) 220228
Fig. 6. Surface aspect of annealed niobium samples: (a) in the start condition (as-polished); and tested for times of (b) 10min; (c) 30min; (d) 50min; (e) 120min; and (f)
the surface aspect of the sample tested for a time of 50min, in higher magnication.
Table 3
Cumulative mass loss (CML) and average erosion rate (AER) as a function of the testing time for niobiumsamples in the cold-worked state and for annealed niobiumsamples
in the C2 condition.
Parameter Niobiumcondition Cavitation time (min)
10 30 40 50 60 70 80 90 100 130
CML (mg)
Cold-worked 0.1 0.2 0.9 3.5 9.8 16.6 24.6 34.2 46.2 89.0
Annealed 0.0 0.3 0.3 0.4 0.4 0.4 0.5 0.5 1.0 5.4
AER (mg/h)
Cold-worked 0.6 0.4 1.3 4.2 9.8 14.2 18.4 22.8 27.7 41.1
Annealed Nb 0.0 0.6 0.4 0.5 0.4 0.3 0.4 0.3 0.6 2.5
(c) Surface characteristics of eroded annealed niobium
Surface aspect of annealed niobium samples in the start con-
dition (as-polished), and tested for times of 10, 50 and 120min is
showninFig. 6. Changes inthe surface morphology canbe observed
even for short testing times, in the case for 10min, since pits and
undulations become apparent (Fig. 6b). The longer the testing time
the higher was the local plastic deformation, resulting in increase
of undulations. As the testing time varies, the undulations present
changes in width as well as in height. This fact is better evidenced
when the results of Fig. 6c and d are confronted. It can be veri-
ed that the eroded surface morphology is signicantly altered for
longer testing times, in the case for 30 and 50min. Table 4 presents
the average values of the Ra and Rz roughness obtained for sur-
faces illustrated in Fig. 6. These results are in accordance with [4],
which conrms that the characteristics of undulation greatly affect
the roughness of the eroded surface. It is also important to keep
in mind that changes in roughness can be frequently associated to
the transitionbetweenthe incubationstage and the maximumero-
sion rate stage, according to [12]. Such characteristic was veried
in the sample tested for a time of 120min (Fig. 6e), whose rough-
ness was considerably increased in relation to the other conditions
comprising shorter testing times. For a testing time of 240min the
Table 4
Average values of the Ra and Rz roughness obtained for the surfaces illustrated in
Fig. 6, which were eroded for different testing times.
Testing time (min) Ra roughness (m) Rz roughness (m)
0 (as-polished) 0.04 0.28
10 0.06 0.30
30 0.20 1.39
50 0.28 2.04
120 0.92 9.11
240 2.70 18.43
S.F. Brunatto et al. / Wear 274275 (2012) 220228 225
roughness was strongly increased (see Table 4); an effect veried
for both the C1 and C2 conditions. The occurrence of craters at sur-
face conrms that the samples meet in the maximumerosion rate
stage, as observed in Fig. 6e.
Fig. 6f shows, in higher magnication, the surface aspect of the
sample tested for a time of 50min. It is evidenced the beginning
of the microcracks nucleation, which occurs after the appearance
of pits and undulations. The formation of microcracks is intensied
as the testing time is increased from 50 to 120min. In the same
way, the formation of craters and the cumulative mass loss are con-
siderably increased as shown for a sample tested during 120min
(Fig. 6e), what concludes the discussion.
Inaddition, the slight mass loss veriedfor samples tested10, 30
and 50min must be discussed. This fact could be explained by the
presence of surface defects at samples surface. Micropores, impu-
rities, and nishing imperfections such as grinding scratches are
some examples which could affect directly the cavitation resis-
tance, since cavitation process is a local phenomenon [33,58].
Thus, alterations in the cavitation resistance in such sites could
be observed. It is important to note that residual stress, micros-
train or surface texture introduced by nishing processes and do
not completely removed prior to testing could greatly inuence
the incubation stage, which gives support to the above mentioned
assumption. As indicated in Table 3 for annealed niobium sam-
ples, cumulative mass loss of 0, 0.3, 0.4, and 0.5mg was veried for
testing time of 10, 30, 50, and 90min, respectively. Aspects of the
surfaces tested in these conditions are presented in Fig. 7 (10min),
Fig. 8 (30min) and Fig. 9 (50min).
Fig. 7 shows in detail a crater formed in the rst cycles for a
sample tested during 10min, which conrms that advanced mate-
rial removal can be veried in very small and specic sites in the
beginning of the cavitationtesting. The surrounding area inrelation
to the specic crater preserves the characteristics of the incuba-
tion stage, presenting pits and undulations, as previously shown
and discussed in Fig. 6b. It is to be noted striations are presented
all over the crater surface. This result indicates that allied to the
work-hardening effect [57], fatigue is also present in the cavitation
failure mechanism of niobium. The fatigue failure mechanism has
been studied by different authors [11,45]. In the ndings of [11], it
was indicated that single impact loads tend to remove many and
small sharply edgedparticles inthe incubationstage, whereas large
striated particles tend to be formed due to cyclic loads during the
acceleration and the maximumerosion rate stages, conrming the
occurrence of fatigue striations.
Fig. 8 shows in detail the surface aspect of the sample tested
during 30min. Surface presents high degree of plastic deforma-
tion and is characterized by undulations, which appear broken into
small particles in some specic sites due to successive impacts. It
can be seen that transgranular microcracks propagate as parallel as
perpendicular to the vibrating surface, describing the initial stage
of crater formation. The typical aspect of debris characterized by
multiple cracks at surface canbe related to the bcc crystalline struc-
ture of the niobium. The assumption is supported by the fact that
as the strain rate increases, the response of the annealed niobium
to applied stress by material ow becomes difcult and results in
the increase of failure tendency. As known, bcc structure is highly
sensitive to strain rate, differently of the fcc one that is a close-
packedstructure andpresents principal slipsystems for occurrence
of plastic deformation, in accordance with Kwok [20].
Fig. 9 shows the surface aspect of the sample tested during
50min. Results conrm that the surface damage is characterized
by the presence of pits, undulations, and the appearance of fatigue
striations inside craters in specic sites. In the highest magnica-
tion SEMmicrograph showing in detail a crater, it is illustrated the
development of the fatigue process along a symmetry line, which
could be a grain boundary of the annealed niobiumsample.
Fig. 7. Details of the eroded surface for testing time of 10min.
Finally, Fig. 10 shows the surface aspect of the sample tested
during 120min. Besides pits and undulations, the surface investi-
gationalsoindicates theoccurrenceof fatiguestriations andcraters,
which are formed in profusion at the considered testing condi-
tion. The intense formation of craters reects that the capacity of
material in absorbing the impact energy and to deform was n-
ished. Consequently, microcracks and craters formation is spread
all over the surface resulting in strong erosion of the sample, which
characterizes that the maximumerosion rate stage was reached.
In short, the above mentioned results indicate that the cavita-
tion erosion mechanismin niobiumoccurs in a sequence of events
comprising the work-hardening effect and the fracture of debris
allied to the effect of fatigue and microcracks formation.
(d) Comparison of the cavitation erosion behaviour:
niobiumsteel
Fig. 11 presents the cumulative mass loss (CML) as a function
of the cavitation erosion time for annealed niobium and ASTM
226 S.F. Brunatto et al. / Wear 274275 (2012) 220228
Fig. 8. Details of the eroded surface for a testing time of 30min.
CA-6NMstainless steel samples, aiming to confront the cavitation
erosion behaviour of both the materials.
It is to be noted that the ASTM CA-6NM martensitic stainless
steel was developed to improve the weldability of conventional
martensitic stainless steels, as veried for example to the ASTM
CA-15 steel. In addition, due to its high hardenability, it is uti-
lized in diverse applications, normally in the manufacturing of
large parts as hydraulic turbine rotors, andpumps andcompressors
components. CA-6NM steel also presents after tempering excel-
lent mechanical properties, such as high tensile strength, high
Fig. 9. Details of the eroded surface for a testing time of 50min.
cavitation erosion resistance and adequate toughness even at low
temperature [5961]. This explains why it was utilized in the
present work for comparison purpose.
Based on the characteristics of the wear regimes shown in
Fig. 11, it was evidenced that: (a) both the materials have similar
incubation period; and (b) annealed niobiumhas worse behaviour
in the maximumerosion rate stage than steel. Considering that the
cavitation behaviour is intrinsically related to the material charac-
teristics, in accordance with [5], and the studied materials present
the same crystalline structure (bcc), the similarities and differences
veried in Fig. 11 are far frombeing fully explained. This fact justi-
es the continuous demand and additional efforts to elucidate the
relations between the material characteristics and the cavitation
erosion behaviour, as veried in the specialized literature.
Table5summarizes theresults obtainedtodeterminethecumu-
lative mass loss (CML) and the average erosion rate (AER) as a
function of the testing time for annealed niobium samples in the
Table 5
Cumulative mass loss (CML) and the average erosion rate (AER) as a function of the testing time for annealed niobiumsamples in the C2 condition and ASTMCA6-NMstainless
steel samples.
Parameter Material Cavitation time (min)
10 20 50 80 120 140 150 230 240
CML (mg)
Annealed Nb 0.0 0.3 0.4 0.5 2.8 11.2 50.4
ASTM CA-6NM 0.0 0.2 0.3 0.8 3.5 13.7
AER (mg/h)
Annealed Nb 0.0 0.9 0.5 0.4 1.4 4.5 12.6
ASTM CA-6NM 0.0 0.6 0.4 0.6 1.5 3.6
S.F. Brunatto et al. / Wear 274275 (2012) 220228 227
Fig. 10. Surface aspects of the sample tested during 120min.
C2 condition and ASTM CA6-NM stainless steel samples. The CML
and AER were 0.2, 0.3, 0.8, 3.5, and 13.7mg, and 0.6, 0.4, 0.6, 1.5,
and 3.6mg/h, for testing times of 20, 50, 80, 140 and 230min, for
ASTM CA6-NM stainless steel samples, respectively. For annealed
Fig. 11. Cumulative mass loss as a function of the cavitation erosion time for
annealed niobiumand ASTMCA-6NMsteel samples.
niobiumin the C2 condition the results were the same as presented
in Table 3.
4. Conclusions
In this work the cavitation erosion behaviour of niobium in
the annealed and cold-worked state was studied. The results for
annealed niobium were compared with the cavitation erosion
behaviour of CA-6NMmartensitic stainless steel, which is a mate-
rial typically utilized for hydraulic turbines manufacturing. The
main conclusions can be listed as follows:

Cold-worked niobium presents smaller cavitation erosion resis-


tance than annealed niobium.

Annealed niobiumand CA-6NMsteel present similar incubation


period and dissimilar maximum erosion rate stage at the con-
sidered wear regimes, being that the annealed niobiumpresents
worse behaviour in the maximumerosion rate stage than steel.

The cavitation erosion failure mechanismin niobiumoccurs in a


sequence of events comprisingthe work-hardeningeffect andthe
fracture of debris allied to the effect of fatigue and microcracks
formation.
Acknowledgments
The authors would like to acknowledge the Brazilian Agency
CNPq (Conselho Nacional de Desenvolvimento Cientco e Tec-
nolgico) for the nancial support, the CBMM (Companhia
Brasileira de Metalurgia e Minerac o) for the niobium supply and
LACTEC-UFPR for the ASTMCA-6NMstainless steel supply.
References
[1] G.W. Stachowiak, A.W. Batchelor, Abrasive, Erosive and Cavitation Wear
Engineering Tribology, 3rd ed., Butterworth-Heinemann, Boston, 2006, pp.
501555.
[2] L. Rayleigh, Onthe pressure developina liquidduring the collapse of a spherical
cavity, Philosophical Magazine VI 34 (1917) 9498.
[3] ASTMStandard Test Method for Cavitation Erosion Using Vibratory Apparatus,
Standard G32-09, 2009.
[4] K.Y. Chiu, F.T. Cheng, H.C. Man, Evolution of surface roughness of some metallic
materials in cavitation erosion, Ultrasonics 43 (2005) 713716.
[5] H.G. Feller, Y. Kharrazi, Cavitation erosion of metals and alloys, Wear 93 (1984)
249260.
[6] Z. Yu-Kang, F.G. Hammitt, Cavitationerosionincubationperiod, Wear 86(1983)
299313.
[7] S.M. Ahmed, K. Hokkirigawa, Y. Ito, R. Oba, Scanningelectronmicroscopyobser-
vation on the incubation period of vibratory cavitation erosion, Wear 142
(1991) 303314.
[8] G.B. Jiang, Y.K. Zheng, Y.Y. Yang, H.S. Fang, Cavitation erosion of bainitic steel,
Wear 215 (1998) 4653.
[9] C.T. Kwok, H.C. Man, F.T. Cheng, Cavitation erosion of duplex and super duplex
stainless steels, Scripta Materialia 39 (1998) 12291236.
[10] W. Bedkowski, G. Gasiak, C. Lachowicz, A. Lichtarowicz, T. Lagoda, E. Macha,
Relations between cavitation erosion resistance of materials and their fatigue
strength under randomloading, Wear 230 (1999) 201209.
[11] S. Hattori, E. Nakao, Cavitationerosionmechanisms andquantitativeevaluation
based on erosion particles, Wear 249 (2001) 839845.
[12] M. Pohl, J. Stella, Quantitative CLSM roughness study on early
cavitationerosion damage, Wear 252 (2002) 501511.
[13] R. Pai, D.J. Hargreaves, Performance of environment-friendly hydraulic uids
and material wear in cavitating conditions, Wear 252 (2002) 970978.
[14] C.J. Lin, J.L. He, Cavitation erosion behavior of electroless nickel-plating on AISI
1045 steel, Wear 259 (2005) 154159.
[15] S.J. Pawel, Assessment of cavitationerosion resistance of 316LNstainless steel
in mercury as a function of surface treatment, Journal of Nuclear Materials 343
(2005) 101115.
[16] R.J. DiMel, Onthe transitiontointergranular fracture during hightemperature
deformation, Materials Science and Engineering A 158 (1992) 5363.
[17] A. Krella, A. Czy zniewski, Inuence of the substrate hardness on the cavitation
erosion resistance of TiN coating, Wear 263 (2007) 395401.
[18] J. Steller, A. Krella, J. Koronowicz, W. Janicki, Towards quantitative assessment
of material resistance to cavitation erosion, Wear 258 (2005) 604613.
[19] S.M. Ahmed, K. Hokkirigawa, R. Oba, Fatigue failure of SUS 304 caused by vibra-
tory cavitation erosion, Wear 177 (1994) 129137.
228 S.F. Brunatto et al. / Wear 274275 (2012) 220228
[20] C.T. Kwok, H.C. Man, F.T. Cheng, Cavitation erosion and damage mechanisms of
alloys with duplex structures, Materials Science and Engineering A 242 (1998)
108120.
[21] A. Karimi, F. Avellan, Comparison of erosion mechanisms in different types of
cavitation, Wear 113 (1986) 305322.
[22] W.J. Tomlinson, N. Kalitsounakis, G. Vekinis, Cavitation erosion of aluminas,
Ceramics International 25 (1999) 331338.
[23] C.T. Kwok, H.C. Man, F.T. Cheng, Cavitation erosion and pitting corrosion
behaviour of laser surface-melted martensitic stainless steel UNS S42000, Sur-
face and Coatings Technology 126 (2000) 238255.
[24] N. Long, J. Zhu, Formation of nanocrystallized and amorphous structures in the
cavitation-eroded surface for Ti
3
AlNb alloy, Materials Science and Engineer-
ing: A 420 (2006) 276278.
[25] M.K. Lee, S.M. Hong, G.H. Kim, K.H. Kim, C.K. Rhee, W.W. Kim, Numerical cor-
relation of the cavitation bubble collapse load and frequency with the pitting
damage of ame quenched Cu9Al4.5Ni4.5Fe alloy, Materials Science and
Engineering A 425 (2006) 1521.
[26] S. Hattori, A. Tainaka, Cavitation erosion of TiNi base shape memory alloys,
Wear 262 (2007) 191197.
[27] H. Mochizuki, M. Yokota, S. Hattori, Effects of materials and solution temper-
atures on cavitation erosion of pure titanium and titanium alloy in seawater,
Wear 262 (2007) 522528.
[28] H. Mindivan, M. Baydogan, E.S. Kayali, H. Cimenoglu, Wear behaviour of 7039
aluminumalloy, Materials Characterization 54 (2005) 263269.
[29] Y. Ichida, R. Sato, Y. Morimoto, K. Kobayashi, Material removal mechanisms in
non-contact ultrasonic abrasive machining, Wear 258 (2005) 107114.
[30] S. Hattori, K. Maeda, Q. Zhang, Formulationof cavitationerosionbehavior based
on logistic analysis, Wear 257 (2004) 10641070.
[31] B.C.S. Rao, D.H. Buckley, Deformation and erosion of F.C.C. metals and alloys
under cavitation attack, Materials Science and Engineering 67 (1984) 5567.
[32] B.C.S. Rao, D.H. Buckley, Erosion of aluminum6061-T6 under cavitation attack
in mineral oil and water, Wear 105 (1985) 171182.
[33] B.C.S. Rao, D.H. Buckley, Scanning electron microscopy investigation of surface
deformation features on -brass single crystals exposed to cavitation attack,
Materials Science and Engineering 76 (1985) L1L5.
[34] R.N. Wright, D.E. Mikkola, Cavitation-induced erosion of ordered and disor-
dered Cu
3
Au, Materials Science and Engineering 26 (1976) 263268.
[35] Y. Meged, Modeling of the initial stage in vibratory cavitation erosion tests by
use of a Weibull distribution, Wear 253 (2002) 914923.
[36] W.J. Tomlinson, S.J. Matthews, Cavitationerosionof structural ceramics, Ceram-
ics International 20 (1994) 201209.
[37] D. Niebuhr, Cavitation erosion behavior of ceramics in aqueous solutions, Wear
263 (2007) 295300.
[38] C. Godoy, R.D. Mancosu, M.M. Lima, D. Brando, J. Housden, J.C. Avelar-Batista,
Inuence of plasma nitriding and PAPVD Cr
1x
Nx coating on the cavitation
erosion resistance of an AISI 1045 steel, Surface and Coatings Technology 200
(2006) 53705378.
[39] B.G. Gire n, M. Szkodo, J. Steller, Cavitationerosionof some laser-producediron-
base corrosion-resistant alloys, Wear 258 (2005) 614622.
[40] C.T. Kwok, F.T. Cheng, H.C. Man, Laser surface modication of UNS S31603
stainless steel. Part II. Cavitation erosion characteristics, Materials Science and
Engineering A 290 (2000) 7488.
[41] F.T. Cheng, C.T. Kwok, H.C. Man, Laser surfacing of S31603 stainless steel with
engineering ceramics for cavitation erosion resistance, Surface and Coatings
Technology 139 (2001) 1424.
[42] W.H. Huang, K.C. Chen, J.L. He, A study on the cavitation resistance of ion-
nitrided steel, Wear 252 (2002) 459466.
[43] C.H. Tang, F.T. Cheng, H.C. Man, Laser surface alloying of a marine pro-
peller bronze using aluminium powder. Part I. Microstructural analysis
and cavitation erosion study, Surface and Coatings Technology 200 (2006)
26022609.
[44] C.H. Tang, F.T. Cheng, H.C. Man, Laser surface alloying of a marine propeller
bronze using aluminiumpowder. Part II. Corrosion and erosioncorrosion syn-
ergism, Surface and Coatings Technology 200 (2006) 25942601.
[45] C.M. Garzn, H. Thomas, J.F. dos Santos, A.P. Tschiptschin, Cavitation erosion
resistanceof a hightemperaturegas nitridedduplexstainless steel insubstitute
ocean water, Wear 259 (2005) 145153.
[46] A. Krella, A. Czy zniewski, Cavitation erosion resistance of CrN coating
deposited on stainless steel, Wear 260 (2006) 13241332.
[47] M. Duraiselvam, R. Galun, V. Wesling, B.L. Mordike, R. Reiter, J. Olig-
mller, Cavitation erosion resistance of AISI 420 martensitic stainless steel
laser-clad with nickel aluminide intermetallic composites and matrix com-
posites with TiC reinforcement, Surface and Coatings Technology 201 (2006)
12891295.
[48] M. Duraiselvam, R. Galun, V. Wesling, B.L. Mordike, R. Reiter, J. Oligmller, G.
Buvanashekaran, Cavitation erosion resistance of Ti6Al4V laser alloyed with
TiC-reinforced dual phase intermetallic matrix composites, Materials Science
and Engineering A 454455 (2007) 6368.
[49] C. Pitsch, B. Curdts, V. Buck, B. Atakan, Wear properties of MOCVD-grown
aluminiumoxide lms studied by cavitation erosion experiments, Surface and
Coatings Technology 201 (2007) 92999303.
[50] ASMInternational HandbookCommittee, ASMHandbook, vol. 2, 10thed., 1990,
p. 565.
[51] W.D. Wilkinson, Fabrication of Refractory Metals, Gordon and Breach Science
Publishers Inc., NewYork/London/Paris, 1970, pp. 184195.
[52] G. Bregliozzi, A. di Schino, S.I.-U. Ahmed, J.M. Kenny, H. Haefke, Cavitation
wear behavior of austenitic stainless steels with different grain sizes, Wear
258 (2005) 503510.
[53] M. Dular, B. Stoffel, B.

Sirok, Development of a cavitation erosion model, Wear
261 (2006) 642655.
[54] R.F. Patella, J.-L. Reboud, A. Archer, Cavitationdamage measurement by3Dlaser
prolometry, Wear 246 (2000) 5967.
[55] E. Samiei, M. Shams, R. Ebrahimi, A novel numerical scheme for the investi-
gation of surface tension effects on growth and collapse stages of cavitation
bubbles, European Journal of Mechanics B/Fluids 30 (2011) 4150.
[56] X. Chen, R.Q. Xu, Z.H. Shen, J. Lu, X.W. Ni, Optical investigation of cavitation
erosion by laser-induced bubble collapse, Optics & Laser Technology 36 (2004)
197203.
[57] N. Berchiche, J.-P. Franc, J.-M. Michel, Un modle de prdiction de lrosion
des matriaux ductiles par la cavitation, Comptes Rendus de lAcadmie des
Sciences, Series IIB: Mechanics-Physics-Astronomy 328 (2000) 305310 (in
French).
[58] X. Zhao, Effect of surface modication processes on cavitation erosion resis-
tance, PhD thesis, Doutorado em Cincia dos Materiais - PIPE - Universidade
Federal do Paran, Brazil, 2002, p. 27.
[59] J.D. Crawford, CA6NM an update, in: Proceedings of the 29th Annual Steel
Founders Society of America Technical and Operating Conference, 1974, pp.
113.
[60] T.G. Gooch, Heat treatment of welding 13%Cr4%Ni martensitic stainless steel
for sour service, Welding Research Supplement July (1995) 213222.
[61] P.D. Bilmes, C.L. Llorente, I.J. Prez, Toughness and microstructure of
13Cr4NiMo high strength steel welds, Journal of Materials Engineering and
Performance 9 (2000) 609615.