Cavitation Erosion Behaviour of Niobium:, A.N. Allenstein, C.L.M. Allenstein, A.J.A. Buschinelli
Cavitation Erosion Behaviour of Niobium:, A.N. Allenstein, C.L.M. Allenstein, A.J.A. Buschinelli
Cavitation Erosion Behaviour of Niobium:, A.N. Allenstein, C.L.M. Allenstein, A.J.A. Buschinelli
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 [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