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International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 466
Taguchi analysis of single layer CrN coatings on
AISI 304 Stainless Steel to study its erosive
corrosive wear behaviour
Alok Vats
M. Tech, Production Engineering, MNIT Jaipur, Pass out 2016
Address: Plot No. 761 Mundka, New Delhi- 110041 (Near Swati Modern Public School)
Abstract— The purpose of present study was to
investigate the erosive corrosive wear behavior of single
layer (CrN) coatings on AISI 304 Stainless Steel samples
with varying coating thickness (0-200 nm) in the range of
50 nm. The slurry jet erosive test was conducted on Slurry
Jet Erosion Tester in saline slurry (3.5wt% salt) under the
different working conditions with varying impact velocity
(10-25 m/s), impingement angle (30°-75°) and erodent
discharge (160-280 gm/min). Taguchi analysis was
applied to find optimum parameters for the minimization
of erosion rate of various coated and uncoated samples.
The results of Taguchi experiments also indicated that
among all the factors, impact velocity became least
significant when samples were coated with CrN whereas
it was most significant for uncoated samples. Coating
thickness was the second most significant factor in the
case of CrN coated samples. PVD- CrN coatings reduced
the wear rate by nearly 2 times.
Keywords— Erosive wear, corrosive wear, single layer
coating, Taguchi Orthogonal Array.
I. INTRODUCTION
Erosion–corrosion is the increase in the rate of
degradation of the material caused by the combined action
of electrochemical corrosion and mechanical wear
processes. Corrosion is a material degradation process
which occurs due to electrochemical action, while erosion
is a mechanical wear process. When these two processes
act together especially in the marine environments, it is
known as erosion-corrosion. It is one of the major causes
of failure in the nuclear power plants, chemical,
petrochemical industries and marine environments where
combined effect of erosion and corrosion phenomena
occurs. In the marine field, this study applies to ship and
boats. The study is equally beneficial in those areas where
the underground salty water is supplied for household
purposes, and the same has to be delivered to the
overhead tank.
In the liquid- particle flow, the sand particles get impinged
on steel surface which remove a layer of protective film
from its surface. The chloride ions act rapidly on the
exposed surface having discontinuity. In this way pure
erosion and erosion enhanced corrosion are the dominant
mechanisms that degrade the metal surface in erosion
corrosion [1-6]. In order to improve the physical,
mechanical and surface wear of metal such as steel,
surface treatment such as modification of surface using
silane, electroplating, Nitriding and coating etc are used
[7-13]. A majority of surface modification lead to
improved corrosive characteristics of the steel. Hence,
they are also called corrosion inhibitors and are used on
variety of steels. Neville et al. [7] studied erosion–
corrosion of engineering steels by the use of chemicals on
X65 pipeline steel, 13Cr martensitic stainless steel and
super-duplex stainless steels. They concluded that
inhibitor has a greater effect on the corrosion component
of carbon steel but offers no protection on super-duplex
stainless steel under the conditions tested. In another
research, Hu et al.[14] assessed the effect of corrosion
inhibitor on erosion–corrosion of API-5L-X65 stainless
steel in multi-phase jet impingement conditions and found
that corrosion inhibitor provides up to 20% protection in
erosion–corrosion conditions and that oil phase reduces
the erosion component by reducing the particle velocity in
the flow conditions. Yao et al. [15] investigated a new
method for protecting bends from erosion in gas-particle
flows and reported that adding ribs on the outer-wall of the
inside bend can significantly improve bend’s erosion
protection ability. Surface coating technology has also
been deployed to enhance the erosive corrosive
characteristics of the metals. Multilayer coatings offer
protection against synergistic effects on bare stainless steel
surfaces.
Corrosion resistance can also be increased by providing
an interlayer of a suitable material [16]. Coatings of CrN
and CrCN have been commonly used in industry and
research to improve surface properties of materials.
However, CrCN coatings provide better corrosion
resistance than CrN coated samples due to its superior
mechanical properties [17]. Shan et al. [18] fabricated
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 467
CrN coatings on 316L stainless steel substrate by multi-
arc ion plating system, performed Polarization tests and
concluded that the multilayer structure could limit the
crack propagation only to the layer and reduce cracks in
the coating. However, there are various other factors
besides the coating thickness that affect the erosive
corrosive performance under practical conditions. These
are impact velocity, impingement angle and erodent
discharge respectively. The erosive corrosive performance
of the material under a given combination of these factors
has not been fully understood.
Hence, the aim of this work was to fabricate single layer
coated AISI 304 stainless steel material, study the effect
of various parameter such as coating thickness, impact
velocity, erodent discharge and impingement angle on the
erosive and corrosive behavior of fabricated material and
finally to find different levels of factors to achieve a
condition of minimum wear rate using Taguchi’s
approach.
II. EXPERIMENTAL PROCEDURE
2.1 Materials
The proposed work consists of deposition of mono-
layered PVD coatings of CrN of varying thickness on
AISI 304 stainless steel. AISI 304 stainless steel was
purchased from Bahubali Steels, New Delhi. While
Chromium powder was procured from M/s Indian
Diamond Tools and M/s Scientific Instruments, Jaipur,
India.
2.2 Sample Preparation and Coating Process
The samples for coating were prepared as per test
standard specification with the help of a diamond cutter.
Then the uncoated samples were mirror-polished using a
MetaServe 250 Grinder Polisher (Buhler machine,
Illinois, USA). The fine polish provides the improvement
of adherence between coating and the samples. Before
coating, samples were cleaned in acetone and then dried
in a pre-vacuum dryer. The pellets used for coating were
prepared with the help of 99.5% pure Cr powder procured
from M/s Indian Diamond Tools and M/s Scientific
Instruments, Jaipur. The pellet were pressed using a KBr
press at a pressure of 15 tonnes.
A thermal Vapor deposition process (inside a high
temperature Vacuum Box Coater -Model BC-300, Hind
High Vacuum Co. (P) Ltd. Bangalore, India) (Figure.1)
was used to fabricate single layer (chromium nitride)
coated AISI 304 Stainless Steel with varying coatings
thickness (50nm, 100nm, 150nm and 200nm). In this
coating process, a sample of AISI 304 Stainless Steel was
first positioned in the sample holder. Then a tungsten
filament was used to hold the pellet of pure chromium. A
high vacuum of 10−3
bar was created inside the chamber
and current (50-75 A, 12 V) was supplied to the tungsten
filament to evaporate pure chromium. Then, nitrogen gas
was allowed to flow in the chamber which reacted with the
evaporated chromium and a layer of chromium nitride was
deposited on the surface of the AISI 304 Stainless Steel.
Coating thickness was maintained as 50nm, 100nm,
150nm and 200nm. Four different coatings were
developed. Parameters for CrN coating were taken as
coating rate- 0.1 Å/sec, coating thickness-200nm, Vacuum
Chamber temperature-2000°C, Vacuum Pressure- 1.2x10-6
bar, Nitrogen flow rate- 50cc/min, Voltage-12V, Current-
39 Ampere.
2.3 Sample characterization
2.3.1 Slurry Jet Erosion Test
The slurry erosion behavior of single layer CrN coated and
uncoated samples was evaluated using a Slurry Jet Erosion
Tester (Model TR411, Ducom, India) (Figure. 2). For this
test, slurry was prepared by mixing sand particles and
water and taken in the hopper. Square samples of
dimensions 25 × 25 mm was placed in the sample holder.
Samples were eroded by flow of erodent discharge
through a nozzle of 4 mm diameter. Impingement angles
were changed by adjusting the sample holder at different
angles (30°, 45°, 60° and 75°). The strike was applied for
10 min. The weight loss was determined by the weighing
the sample before and after the slurry erosion test. The
slurry erosion rate was calculated by dividing weight loss
of samples with the time taken to perform an experiment
i.e. 10min.
2.3.2 Design of Experiment (DOE)
Taguchi orthogonal Design of Experiment is one of the
most important and highly beneficial statistical tools and
is employed to examine the effect of more than one
variable and their interactions on the output of the
process. It involves a large number of steps in series
which follow a definite sequence for the test conducted to
provide an improved solution. S/N ratio is the main
quantity that has to be calculated in DOE to obtain an
improved solution. The S/N ratio is calculated using Eq.
(1) as below:
𝑆/𝑁 = 10 𝑙𝑜𝑔 [
1
𝑛
∑ 𝑦𝑖
2𝑛
𝑖=1 ] Eq. (1)
Where, n is the number of tests and yi is the value of
experimental result of the ith
test. The characteristics of
S/N ratio have been categorized into three classes, i.e.
smaller-the-better, larger-the-better, and nominal-the-
better. For obtaining optimal and improved performance,
smaller-the-better characteristic has been selected for
erosion wear. Table 1 indicates the factors selected for
experimental analysis using Taguchi method. The array
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 468
chosen in this study was L16 orthogonal array design
which has 16 rows corresponding to the number of
variables selected.
Table.1: Levels of the variables used in the experiment
Control factors
Levels
1 2 3 4 Units
Coating thickness (A) 50 100 150 200 nm
Impact velocity (B) 10 15 20 25 m/s
Impingement angle (C) 30 45 60 75 degree
Erodent discharge (D) 160 200 240 280 gm/min
III. RESULTS AND DISCUSSION
3.1 Wear Characteristic analysis by Taguchi method
3.1.1 For single layer (CrN) coatings of various
thicknesses (50nm, 100nm, 150nm and 200nm) on AISI
304 Stainless Steel
The experiments were performed as per Taguchi
Orthogonal L16 array. In Table 2, seventh column
represents S/N ratio of the volumetric wear rate of the
coated samples. The overall mean for the S/N ratio of the
specific wear rate was found to be 56.097 db for the
coated samples. The analysis was performed using the
software MINITAB 17 to analyze the wear rate of the
coated samples. Table 4 indicated that that among various
factors, erodent discharge is the most significant factor
followed by coating thickness and impingement angle.
Impact velocity has the least significance on erosion rate
of the CrN coated 304 steel.
On the other hand, Table 3 revealed that uncoated 304
steel indicated more wear than the coated steel. The mean
wear rate in Table 3 (0.0033103gm/min) was more than
that in Table 2 (0.001656 gm/min). It means that PVD-
CrN coating reduced the wear rate by nearly 2 times. The
improvement in wear resistance due to PVD coating on
AISI 304 stainless steel was also observed by Recco et al.
[13]. They concluded that PVD-TiN coating reduced the
wear rate by 20 times. Analysis of the results from Figure
3 leads to the conclusion that combination of factors A4,
B4, C2 and D2 gives minimum erosion rate. Hence, the
optimum parameter for the minimum wear rate was at
coating thickness 200nm, maximum impact velocity
25m/sec, and impingement angle of 45° and erodent
discharge of 280 gm/min.
Fig.3: Influence of control factors on the Erosion rate of single layer (CrN) coatings of various thicknesses (50nm, 100nm,
150nm and 200nm) on AISI 304 Stainless Steel
3.1.2 For uncoated 304 Stainless Steel
The experimental results for uncoated 304 Stainless Steel
were also analyzed by Taguchi method. The following
results were obtained in which the overall mean for S/N
ratio of erosion rate is 50.263. The erosion rate and S/N
ratio responses were presented in Table 3 from which it
can be concluded that impact velocity was the most
significant factor followed by impingement angle.
However, erodent discharge has indicated the least
significance on erosion rate of the uncoated 304 steel.
Further, Figure 4 concluded that combination of factors
B4, C4 and D2 gives minimum erosion rate. Hence,
optimum parameters for the minimum erosion rate of
uncoated SS-304 were found to be Impact velocity of
25m/sec, impingement angle of 45° and erodent discharge
of 240gm/min.
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 469
Table.2: Experimental design using L16 orthogonal array for CrN coated 304 steel
S. No. Coating
thickness
(nm)
Impact
velocity
(m/sec)
Impingement
angle
(degrees)
Erodent
discharge
(gm/min)
Erosion rate
(gm/min)
S/N
Ratio
(db)
1 50 10 30 160 0.0024 52.3958
2 50 15 45 200 0.0017 55.3910
3 50 20 60 240 0.0030 50.4576
4 50 25 75 280 0.0016 55.9176
5 100 10 45 240 0.0018 54.8945
6 100 15 30 280 0.0020 53.9794
7 100 20 75 160 0.0014 57.0774
8 100 25 60 200 0.0012 58.4164
9 150 10 60 280 0.0011 59.1721
10 150 15 75 240 0.0026 51.7005
11 150 20 30 200 0.0013 57.7211
12 150 25 45 160 0.0012 58.4164
13 200 10 75 200 0.0010 60.0000
14 200 15 60 160 0.0012 58.4164
15 200 20 45 280 0.0011 59.1721
16 200 25 30 240 0.0019 54.4249
Mean wear rate 0.001656 50.097
Table.3: Experimental design using L16 orthogonal array for AISI 304 steel
S. No. Impact
velocity
(m/sec)
Impingement
angle
(degrees)
Erodent
discharge
(gm/min)
Erosion rate
(gm/min)
S/N
Ratio
(db)
1 10 30 160 0.00400 47.9588
2 10 45 200 0.00360 48.8739
3 10 60 240 0.00370 48.6360
4 10 75 280 0.00380 48.4043
5 15 30 200 0.00340 49.3704
6 15 45 160 0.00310 50.1728
7 15 60 280 0.00330 49.6297
8 15 75 240 0.00290 50.7520
9 20 30 240 0.00280 51.0568
10 20 45 280 0.00310 50.1728
11 20 60 160 0.00260 51.7005
12 20 75 200 0.00270 51.3727
13 25 30 280 0.00300 50.4576
14 25 45 240 0.00275 51.2133
15 25 60 200 0.00240 52.3958
16 25 75 160 0.00250 52.0412
Mean wear rate 0.0033103 50.2630
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 470
25201510
51
50
49
75604530
280240200160
51
50
49
impact velocityMeanofSNratios impingement angle
erodent discharge
Main Effects Plot for SN ratios
Data Means
Signal-to-noise: Smaller is better
Fig.4: Effect of control factors on the Erosion rate uncoated AISI 304 Stainless Steel
3.2 ANOVA Analysis
Analysis of variance (ANOVA) was used to investigate
the influence of various input parameters like impact
velocity, impingement angle and erodent discharge on the
basis of experimental results. By ANOVA analysis we
determined the percentage contribution of that particular
variable and its dominance over other factors. Table 4
presented ANOVA results for erosion rate for single layer
(CrN) coatings of various thicknesses (50nm, 100nm,
150nm and 200nm) on AISI 304 Stainless Steel the
erodent discharge (46.14 %), coating thickness (33.13 %),
impact velocity (7.05 %), and impingement angle (9.95 %)
have an influence on the saline slurry erosion rate. Out of
these factors, erodent discharge indicated the most
significant factor for the saline slurry erosion wear and
impact velocity indicated as the least significant factor in
the case of slurry erosion rate for single layer CrN
coatings of various thicknesses (50nm, 100nm, 150nm and
200nm) on AISI 304 Stainless Steel. On the other hand,
Table 5 indicated ANOVA analysis for uncoated SS304
steel alloy having 3 factors, 4 levels and interaction of
those factors. It can be revealed that the impact velocity
(81.22 %), impingement angle (8.4764 %) and erodent
discharge (7.01%) have an influence on the saline slurry
erosion rate. Out of these factors, impact velocity was
considered as the most significant factor for the saline
slurry erosion of the uncoated 304 steel samples and
erodent discharge is the least significant factor in the case
of slurry erosion rate for uncoated 304 steel. This result
was in agreement with Gautam et al. [19] who obtained
impact velocity (79.85%) as the most significant factor in
case of uncoated granite powder reinforced composites.
Therefore, from both the Table 4 and 5 it can be seen that
for uncoated sample impact velocity has most significant
effect on erosion rate whereas it has least significant effect
for CrN coated AISI 304 Stainless Steel. Hence, it can be
concluded that for the application where velocity of slurry
and water is high, thicker the single layer coating of CrN
on AISI 304 Stainless Steel the more effective it will be.
Table.4: ANOVA table for Erosion rate of single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and
200nm) on AISI 304 Stainless Steel
Source DF AdjSS Adj MS F-Value P-Value
coating thickness 3 42.399 14.133 8.91 0.053
impact velocity 3 9.023 3.008 1.90 0.306
impingement angle 3 12.742 4.247 2.68 0.220
erodent discharge 3 59.048 19.683 12.41 0.034
Error 3 4.760 1.587
Total 15 127.972
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 471
Table.5: ANOVA table for uncoated AISI 304 stainless steel
Source DF Seq SS Adj SS Adj MS F P
impact velocity 3 22.2345 22.2345 7.4115 49.28 0.000
impingement angle 3 2.3204 2.3204 0.7735 5.14 0.043
erodent discharge 3 1.9165 1.9165 0.6388 4.25 0.063
Error 6 0.9025 0.9025 0.1504
Total 15 27.3738
IV. CONCLUSIONS
The following conclusions can be drawn on the basis of
erosive corrosive wear of the single layer (CrN) coatings
of various thicknesses (50nm, 100nm, 150nm and 200nm)
on AISI 304 Stainless Steel and uncoated 304 steel by
setting the various parameters such as coating thickness,
impact velocity, impingement angle and erodent discharge
at significant levels:
1. Impact velocity was the most significant factor for
uncoated AISI 304 steel sample whereas it indicated
least significance for single layer CrN coated AISI
304 steel samples. However, for coated material,
erodent discharge was the most significant factor,
followed by coating thickness in the erosive
corrosive wear of the CrN coated samples.
2. Analysis of the results for CrN coated 304 steel
samples leads to the conclusion that combination of
factors A4, B4, C2 and D2 gives minimum erosion
rate. Hence, the optimum parameter for the minimum
wear rate was at coating thickness 200nm, maximum
impact velocity 25m/sec, and impingement angle of
45° and erodent discharge of 280 gm/min.
3. Combination of factors B4, C4 and D2 gives
minimum erosion rate in case of uncoated steel.
Hence, optimum parameters for the minimum
erosion rate of uncoated SS-304 were found to be
Impact velocity of 25m/sec, impingement angle of
45° and erodent discharge of 240gm/min. Erodent
discharge has indicated the least significance on
erosion rate of the uncoated 304 steel
4. Results also revealed that uncoated 304 steel
indicated more wear than the coated steel. The mean
wear rate in uncoated 304 steel (0.0033103gm/min)
was more than that in CrN coated 304 steel
(0.001656 gm/min). It means that PVD- CrN coating
reduced the wear rate by nearly 2 times. Hence, for
the application having high flow of water coated
samples should be preferred over uncoated samples.
Fig.2: Test setup of Slurry Jet Erosion Tester
International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 472
Fig.1: Thermal/E-beam PVD Coating Unit
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International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017]
https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311
www.ijaems.com Page | 473
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[19]Shan, L., Wang, Y., Li, J., Jiang, X., Chen, J. (2015)
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[20]Gautam, V., Patnaik, A., Bhat, I. K. (2016)
Microstructure and Wear Behavior of Single layer
(CrN) and Multilayered (SiN/CrN) Coatings on
Particulate Filled Aluminum Alloy Composites,
Silicon DOI 10.1007/s12633-015-9357-9.

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Taguchi analysis of single layer CrN coatings on AISI 304 Stainless Steel to study its erosive corrosive wear behaviour

  • 1. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 466 Taguchi analysis of single layer CrN coatings on AISI 304 Stainless Steel to study its erosive corrosive wear behaviour Alok Vats M. Tech, Production Engineering, MNIT Jaipur, Pass out 2016 Address: Plot No. 761 Mundka, New Delhi- 110041 (Near Swati Modern Public School) Abstract— The purpose of present study was to investigate the erosive corrosive wear behavior of single layer (CrN) coatings on AISI 304 Stainless Steel samples with varying coating thickness (0-200 nm) in the range of 50 nm. The slurry jet erosive test was conducted on Slurry Jet Erosion Tester in saline slurry (3.5wt% salt) under the different working conditions with varying impact velocity (10-25 m/s), impingement angle (30°-75°) and erodent discharge (160-280 gm/min). Taguchi analysis was applied to find optimum parameters for the minimization of erosion rate of various coated and uncoated samples. The results of Taguchi experiments also indicated that among all the factors, impact velocity became least significant when samples were coated with CrN whereas it was most significant for uncoated samples. Coating thickness was the second most significant factor in the case of CrN coated samples. PVD- CrN coatings reduced the wear rate by nearly 2 times. Keywords— Erosive wear, corrosive wear, single layer coating, Taguchi Orthogonal Array. I. INTRODUCTION Erosion–corrosion is the increase in the rate of degradation of the material caused by the combined action of electrochemical corrosion and mechanical wear processes. Corrosion is a material degradation process which occurs due to electrochemical action, while erosion is a mechanical wear process. When these two processes act together especially in the marine environments, it is known as erosion-corrosion. It is one of the major causes of failure in the nuclear power plants, chemical, petrochemical industries and marine environments where combined effect of erosion and corrosion phenomena occurs. In the marine field, this study applies to ship and boats. The study is equally beneficial in those areas where the underground salty water is supplied for household purposes, and the same has to be delivered to the overhead tank. In the liquid- particle flow, the sand particles get impinged on steel surface which remove a layer of protective film from its surface. The chloride ions act rapidly on the exposed surface having discontinuity. In this way pure erosion and erosion enhanced corrosion are the dominant mechanisms that degrade the metal surface in erosion corrosion [1-6]. In order to improve the physical, mechanical and surface wear of metal such as steel, surface treatment such as modification of surface using silane, electroplating, Nitriding and coating etc are used [7-13]. A majority of surface modification lead to improved corrosive characteristics of the steel. Hence, they are also called corrosion inhibitors and are used on variety of steels. Neville et al. [7] studied erosion– corrosion of engineering steels by the use of chemicals on X65 pipeline steel, 13Cr martensitic stainless steel and super-duplex stainless steels. They concluded that inhibitor has a greater effect on the corrosion component of carbon steel but offers no protection on super-duplex stainless steel under the conditions tested. In another research, Hu et al.[14] assessed the effect of corrosion inhibitor on erosion–corrosion of API-5L-X65 stainless steel in multi-phase jet impingement conditions and found that corrosion inhibitor provides up to 20% protection in erosion–corrosion conditions and that oil phase reduces the erosion component by reducing the particle velocity in the flow conditions. Yao et al. [15] investigated a new method for protecting bends from erosion in gas-particle flows and reported that adding ribs on the outer-wall of the inside bend can significantly improve bend’s erosion protection ability. Surface coating technology has also been deployed to enhance the erosive corrosive characteristics of the metals. Multilayer coatings offer protection against synergistic effects on bare stainless steel surfaces. Corrosion resistance can also be increased by providing an interlayer of a suitable material [16]. Coatings of CrN and CrCN have been commonly used in industry and research to improve surface properties of materials. However, CrCN coatings provide better corrosion resistance than CrN coated samples due to its superior mechanical properties [17]. Shan et al. [18] fabricated
  • 2. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 467 CrN coatings on 316L stainless steel substrate by multi- arc ion plating system, performed Polarization tests and concluded that the multilayer structure could limit the crack propagation only to the layer and reduce cracks in the coating. However, there are various other factors besides the coating thickness that affect the erosive corrosive performance under practical conditions. These are impact velocity, impingement angle and erodent discharge respectively. The erosive corrosive performance of the material under a given combination of these factors has not been fully understood. Hence, the aim of this work was to fabricate single layer coated AISI 304 stainless steel material, study the effect of various parameter such as coating thickness, impact velocity, erodent discharge and impingement angle on the erosive and corrosive behavior of fabricated material and finally to find different levels of factors to achieve a condition of minimum wear rate using Taguchi’s approach. II. EXPERIMENTAL PROCEDURE 2.1 Materials The proposed work consists of deposition of mono- layered PVD coatings of CrN of varying thickness on AISI 304 stainless steel. AISI 304 stainless steel was purchased from Bahubali Steels, New Delhi. While Chromium powder was procured from M/s Indian Diamond Tools and M/s Scientific Instruments, Jaipur, India. 2.2 Sample Preparation and Coating Process The samples for coating were prepared as per test standard specification with the help of a diamond cutter. Then the uncoated samples were mirror-polished using a MetaServe 250 Grinder Polisher (Buhler machine, Illinois, USA). The fine polish provides the improvement of adherence between coating and the samples. Before coating, samples were cleaned in acetone and then dried in a pre-vacuum dryer. The pellets used for coating were prepared with the help of 99.5% pure Cr powder procured from M/s Indian Diamond Tools and M/s Scientific Instruments, Jaipur. The pellet were pressed using a KBr press at a pressure of 15 tonnes. A thermal Vapor deposition process (inside a high temperature Vacuum Box Coater -Model BC-300, Hind High Vacuum Co. (P) Ltd. Bangalore, India) (Figure.1) was used to fabricate single layer (chromium nitride) coated AISI 304 Stainless Steel with varying coatings thickness (50nm, 100nm, 150nm and 200nm). In this coating process, a sample of AISI 304 Stainless Steel was first positioned in the sample holder. Then a tungsten filament was used to hold the pellet of pure chromium. A high vacuum of 10−3 bar was created inside the chamber and current (50-75 A, 12 V) was supplied to the tungsten filament to evaporate pure chromium. Then, nitrogen gas was allowed to flow in the chamber which reacted with the evaporated chromium and a layer of chromium nitride was deposited on the surface of the AISI 304 Stainless Steel. Coating thickness was maintained as 50nm, 100nm, 150nm and 200nm. Four different coatings were developed. Parameters for CrN coating were taken as coating rate- 0.1 Å/sec, coating thickness-200nm, Vacuum Chamber temperature-2000°C, Vacuum Pressure- 1.2x10-6 bar, Nitrogen flow rate- 50cc/min, Voltage-12V, Current- 39 Ampere. 2.3 Sample characterization 2.3.1 Slurry Jet Erosion Test The slurry erosion behavior of single layer CrN coated and uncoated samples was evaluated using a Slurry Jet Erosion Tester (Model TR411, Ducom, India) (Figure. 2). For this test, slurry was prepared by mixing sand particles and water and taken in the hopper. Square samples of dimensions 25 × 25 mm was placed in the sample holder. Samples were eroded by flow of erodent discharge through a nozzle of 4 mm diameter. Impingement angles were changed by adjusting the sample holder at different angles (30°, 45°, 60° and 75°). The strike was applied for 10 min. The weight loss was determined by the weighing the sample before and after the slurry erosion test. The slurry erosion rate was calculated by dividing weight loss of samples with the time taken to perform an experiment i.e. 10min. 2.3.2 Design of Experiment (DOE) Taguchi orthogonal Design of Experiment is one of the most important and highly beneficial statistical tools and is employed to examine the effect of more than one variable and their interactions on the output of the process. It involves a large number of steps in series which follow a definite sequence for the test conducted to provide an improved solution. S/N ratio is the main quantity that has to be calculated in DOE to obtain an improved solution. The S/N ratio is calculated using Eq. (1) as below: 𝑆/𝑁 = 10 𝑙𝑜𝑔 [ 1 𝑛 ∑ 𝑦𝑖 2𝑛 𝑖=1 ] Eq. (1) Where, n is the number of tests and yi is the value of experimental result of the ith test. The characteristics of S/N ratio have been categorized into three classes, i.e. smaller-the-better, larger-the-better, and nominal-the- better. For obtaining optimal and improved performance, smaller-the-better characteristic has been selected for erosion wear. Table 1 indicates the factors selected for experimental analysis using Taguchi method. The array
  • 3. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 468 chosen in this study was L16 orthogonal array design which has 16 rows corresponding to the number of variables selected. Table.1: Levels of the variables used in the experiment Control factors Levels 1 2 3 4 Units Coating thickness (A) 50 100 150 200 nm Impact velocity (B) 10 15 20 25 m/s Impingement angle (C) 30 45 60 75 degree Erodent discharge (D) 160 200 240 280 gm/min III. RESULTS AND DISCUSSION 3.1 Wear Characteristic analysis by Taguchi method 3.1.1 For single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel The experiments were performed as per Taguchi Orthogonal L16 array. In Table 2, seventh column represents S/N ratio of the volumetric wear rate of the coated samples. The overall mean for the S/N ratio of the specific wear rate was found to be 56.097 db for the coated samples. The analysis was performed using the software MINITAB 17 to analyze the wear rate of the coated samples. Table 4 indicated that that among various factors, erodent discharge is the most significant factor followed by coating thickness and impingement angle. Impact velocity has the least significance on erosion rate of the CrN coated 304 steel. On the other hand, Table 3 revealed that uncoated 304 steel indicated more wear than the coated steel. The mean wear rate in Table 3 (0.0033103gm/min) was more than that in Table 2 (0.001656 gm/min). It means that PVD- CrN coating reduced the wear rate by nearly 2 times. The improvement in wear resistance due to PVD coating on AISI 304 stainless steel was also observed by Recco et al. [13]. They concluded that PVD-TiN coating reduced the wear rate by 20 times. Analysis of the results from Figure 3 leads to the conclusion that combination of factors A4, B4, C2 and D2 gives minimum erosion rate. Hence, the optimum parameter for the minimum wear rate was at coating thickness 200nm, maximum impact velocity 25m/sec, and impingement angle of 45° and erodent discharge of 280 gm/min. Fig.3: Influence of control factors on the Erosion rate of single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel 3.1.2 For uncoated 304 Stainless Steel The experimental results for uncoated 304 Stainless Steel were also analyzed by Taguchi method. The following results were obtained in which the overall mean for S/N ratio of erosion rate is 50.263. The erosion rate and S/N ratio responses were presented in Table 3 from which it can be concluded that impact velocity was the most significant factor followed by impingement angle. However, erodent discharge has indicated the least significance on erosion rate of the uncoated 304 steel. Further, Figure 4 concluded that combination of factors B4, C4 and D2 gives minimum erosion rate. Hence, optimum parameters for the minimum erosion rate of uncoated SS-304 were found to be Impact velocity of 25m/sec, impingement angle of 45° and erodent discharge of 240gm/min.
  • 4. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 469 Table.2: Experimental design using L16 orthogonal array for CrN coated 304 steel S. No. Coating thickness (nm) Impact velocity (m/sec) Impingement angle (degrees) Erodent discharge (gm/min) Erosion rate (gm/min) S/N Ratio (db) 1 50 10 30 160 0.0024 52.3958 2 50 15 45 200 0.0017 55.3910 3 50 20 60 240 0.0030 50.4576 4 50 25 75 280 0.0016 55.9176 5 100 10 45 240 0.0018 54.8945 6 100 15 30 280 0.0020 53.9794 7 100 20 75 160 0.0014 57.0774 8 100 25 60 200 0.0012 58.4164 9 150 10 60 280 0.0011 59.1721 10 150 15 75 240 0.0026 51.7005 11 150 20 30 200 0.0013 57.7211 12 150 25 45 160 0.0012 58.4164 13 200 10 75 200 0.0010 60.0000 14 200 15 60 160 0.0012 58.4164 15 200 20 45 280 0.0011 59.1721 16 200 25 30 240 0.0019 54.4249 Mean wear rate 0.001656 50.097 Table.3: Experimental design using L16 orthogonal array for AISI 304 steel S. No. Impact velocity (m/sec) Impingement angle (degrees) Erodent discharge (gm/min) Erosion rate (gm/min) S/N Ratio (db) 1 10 30 160 0.00400 47.9588 2 10 45 200 0.00360 48.8739 3 10 60 240 0.00370 48.6360 4 10 75 280 0.00380 48.4043 5 15 30 200 0.00340 49.3704 6 15 45 160 0.00310 50.1728 7 15 60 280 0.00330 49.6297 8 15 75 240 0.00290 50.7520 9 20 30 240 0.00280 51.0568 10 20 45 280 0.00310 50.1728 11 20 60 160 0.00260 51.7005 12 20 75 200 0.00270 51.3727 13 25 30 280 0.00300 50.4576 14 25 45 240 0.00275 51.2133 15 25 60 200 0.00240 52.3958 16 25 75 160 0.00250 52.0412 Mean wear rate 0.0033103 50.2630
  • 5. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 470 25201510 51 50 49 75604530 280240200160 51 50 49 impact velocityMeanofSNratios impingement angle erodent discharge Main Effects Plot for SN ratios Data Means Signal-to-noise: Smaller is better Fig.4: Effect of control factors on the Erosion rate uncoated AISI 304 Stainless Steel 3.2 ANOVA Analysis Analysis of variance (ANOVA) was used to investigate the influence of various input parameters like impact velocity, impingement angle and erodent discharge on the basis of experimental results. By ANOVA analysis we determined the percentage contribution of that particular variable and its dominance over other factors. Table 4 presented ANOVA results for erosion rate for single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel the erodent discharge (46.14 %), coating thickness (33.13 %), impact velocity (7.05 %), and impingement angle (9.95 %) have an influence on the saline slurry erosion rate. Out of these factors, erodent discharge indicated the most significant factor for the saline slurry erosion wear and impact velocity indicated as the least significant factor in the case of slurry erosion rate for single layer CrN coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel. On the other hand, Table 5 indicated ANOVA analysis for uncoated SS304 steel alloy having 3 factors, 4 levels and interaction of those factors. It can be revealed that the impact velocity (81.22 %), impingement angle (8.4764 %) and erodent discharge (7.01%) have an influence on the saline slurry erosion rate. Out of these factors, impact velocity was considered as the most significant factor for the saline slurry erosion of the uncoated 304 steel samples and erodent discharge is the least significant factor in the case of slurry erosion rate for uncoated 304 steel. This result was in agreement with Gautam et al. [19] who obtained impact velocity (79.85%) as the most significant factor in case of uncoated granite powder reinforced composites. Therefore, from both the Table 4 and 5 it can be seen that for uncoated sample impact velocity has most significant effect on erosion rate whereas it has least significant effect for CrN coated AISI 304 Stainless Steel. Hence, it can be concluded that for the application where velocity of slurry and water is high, thicker the single layer coating of CrN on AISI 304 Stainless Steel the more effective it will be. Table.4: ANOVA table for Erosion rate of single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel Source DF AdjSS Adj MS F-Value P-Value coating thickness 3 42.399 14.133 8.91 0.053 impact velocity 3 9.023 3.008 1.90 0.306 impingement angle 3 12.742 4.247 2.68 0.220 erodent discharge 3 59.048 19.683 12.41 0.034 Error 3 4.760 1.587 Total 15 127.972
  • 6. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 471 Table.5: ANOVA table for uncoated AISI 304 stainless steel Source DF Seq SS Adj SS Adj MS F P impact velocity 3 22.2345 22.2345 7.4115 49.28 0.000 impingement angle 3 2.3204 2.3204 0.7735 5.14 0.043 erodent discharge 3 1.9165 1.9165 0.6388 4.25 0.063 Error 6 0.9025 0.9025 0.1504 Total 15 27.3738 IV. CONCLUSIONS The following conclusions can be drawn on the basis of erosive corrosive wear of the single layer (CrN) coatings of various thicknesses (50nm, 100nm, 150nm and 200nm) on AISI 304 Stainless Steel and uncoated 304 steel by setting the various parameters such as coating thickness, impact velocity, impingement angle and erodent discharge at significant levels: 1. Impact velocity was the most significant factor for uncoated AISI 304 steel sample whereas it indicated least significance for single layer CrN coated AISI 304 steel samples. However, for coated material, erodent discharge was the most significant factor, followed by coating thickness in the erosive corrosive wear of the CrN coated samples. 2. Analysis of the results for CrN coated 304 steel samples leads to the conclusion that combination of factors A4, B4, C2 and D2 gives minimum erosion rate. Hence, the optimum parameter for the minimum wear rate was at coating thickness 200nm, maximum impact velocity 25m/sec, and impingement angle of 45° and erodent discharge of 280 gm/min. 3. Combination of factors B4, C4 and D2 gives minimum erosion rate in case of uncoated steel. Hence, optimum parameters for the minimum erosion rate of uncoated SS-304 were found to be Impact velocity of 25m/sec, impingement angle of 45° and erodent discharge of 240gm/min. Erodent discharge has indicated the least significance on erosion rate of the uncoated 304 steel 4. Results also revealed that uncoated 304 steel indicated more wear than the coated steel. The mean wear rate in uncoated 304 steel (0.0033103gm/min) was more than that in CrN coated 304 steel (0.001656 gm/min). It means that PVD- CrN coating reduced the wear rate by nearly 2 times. Hence, for the application having high flow of water coated samples should be preferred over uncoated samples. Fig.2: Test setup of Slurry Jet Erosion Tester
  • 7. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 472 Fig.1: Thermal/E-beam PVD Coating Unit REFERENCES [1] Zhang, G. A., Xu, L. Y., Cheng, Y. F. (2009) Investigation of erosion–corrosion of 3003 aluminum alloy in ethylene glycol–water solution by impingement jet system, Corros. Sci. 51, pp 283–290. [2] Shrestha, S., Hodgkiess, T., Neville, A. (2005) Erosion-corrosion behavior of high-velocity oxy- fuel Ni—Cr—Mo—Si—B coatings under high- velocity seawater jet impingement, Wear 259, pp 208–218 [3] Saha, G. C., Khan, T. I. G. A. Zhang, (2011), Erosion–corrosion resistance of microcrystalline and near-nanocrystalline WC–17Co high velocity oxy-fuel thermal spray coatings, Corros. Sci. 53, pp 2106–2114. [4] Hong, S., Wu, Y., Zhang, J., Zheng, Y., Qin, Y., Lin, J. (2015), Effect of ultrasonic cavitation erosion on corrosion behavior of high-velocity oxygen-fuel (HVOF) sprayed near-nanostructured WC-10Co-4Cr coating, Ultrason. Sonochem. 27, pp 374–378. [5] Zhao, Y., Zhou, F., Yao, J., Dong, S., Li, N., (2015), Erosion–corrosion behaviour and corrosion resistance of AISI 316 stainless steel in flow jet impingement, Wear 328-329, pp 464–474. [6] Lin, C. K., Hsu, C. H., Cheng, Y. H., Liang, O. K., Lee, S. L. (2015), A study on the corrosion and erosion behavior of electroless nickel and TiAlN/ZrN duplex coatings on ductile iron, Appl. Surf. Sci. 324, pp 13–19. [7] Neville, A., Wang, C. (2009), Erosion–corrosion of engineering steels—Can it be managed by use of chemicals, Wear 267, pp 2018–2026. [8] Pantoja, M., Abenojar, J., Martínez, M. A., Velasco, F. (2016), Silane pretreatment of electrogalvanized steels: Effect on adhesive properties, International Journal of Adhesion and Adhesives 65, pp 54-62. [9] Pantoja, M., Martínez, M. A., Abenojar, J., Encinas, N., Ballesteros, Y. (2011), Effect of EtOH/H2O ratio and pH on bis-sulfur silane solutions for electrogalvanized steel joints based on anaerobic adhesives, The Journal of Adhesion 87 (7-8), pp 688-708. [10]Martinez, M. A., Calabrés, R., Abenojar, J., Velasco, F., (2008), Sintered High Carbon Steels: Effect of Thermomechanical Treatments on their Mechanical and Wear Performance, Materials Science Forum 591, pp 271-276. [11]Pantoja, M., Martínez, M. A., Abenojar, J., Velasco, F., Real, J. C. (2010), Structural and mechanical characterization of γ- methacryloxypropyltrimethoxysilane (MPS) on Zn- electrocoated steel Journal of Adhesion Science and Technology 24 (11-12), pp 1885-1901. [12]Pantoja, M., Velasco, F., Broekema, D., Abenojar, J., Real, J. C. (2011), The influence of pH on the hydrolysis process of y- methacryloxypropyltrimethoxysilane, analyzed by FT-IR, and the silanization of electrogalvanized
  • 8. International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-5, May- 2017] https://dx.doi.org/10.24001/ijaems.3.5.10 ISSN: 2454-1311 www.ijaems.com Page | 473 steel, Journal of Adhesion Science and Technology 24(6), pp 1131-1143. [13]Recco, A. A., Lopez, C. D., Bevilacqua, A. F., da Silva, F., Tschiptschin, A. P. (2007), [14]Improvement of the slurry erosion resistance of an austenitic stainless steel with combinations of surface treatments: Nitriding and TiN coating, Surf. Coat. Tech. 202, pp 993–997. [15]Hu, X., Alzawai, K., Gnanavelu, A., Neville, A., Wang, C., Crossland, A., Martin, J. (2011), Assessing the effect of corrosion inhibitor on erosion–corrosion of API-5L-X65 in multi-phase jet impingement conditions, Wear 271, pp 1432– 1437. [16]Yao, J., Zhang, B. Z., Fan, J. R. (2000), Investigation of a new protection method for protecting tube from erosion in gas-particle flows, J. Therm. Sci. 9(2), pp 158-162. [17]Wood, R. J. K. (2007) Tribo-corrosion of coatings: a review, J. Phys. D. Appl. Phys. 40(18), pp 5502- 5521. [18]Ye, Y., Wang, Y., Chen, H., Li, J., Yao, Y. (2015) Doping carbon to improve the tribological performance of CrN coatings in seawater, Tribol. Int. 90, pp 362–371. [19]Shan, L., Wang, Y., Li, J., Jiang, X., Chen, J. (2015) Improving tribological performance of CrN coatings in seawater by structure design, Tribol. Int. 8278–88. [20]Gautam, V., Patnaik, A., Bhat, I. K. (2016) Microstructure and Wear Behavior of Single layer (CrN) and Multilayered (SiN/CrN) Coatings on Particulate Filled Aluminum Alloy Composites, Silicon DOI 10.1007/s12633-015-9357-9.