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Title: Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel

Coated with Pack Boriding Method

Authors: Ersan MERTGENÇ

Recieved: 2019-12-16 09:09:25
Accepted: 2020-03-25 21:29:34

Article Type: Research Article

Volume: 24
Issue: 3
Month: June
Year: 2020
Pages: 521-530

How to cite
Ersan MERTGENÇ; (2020), Examination of Wear and Rockwell-C Adhesion Properties
of Nitronic 50 Steel Coated with Pack Boriding Method. Sakarya University
Journal of Science, 24(3), 521-530, DOI:
https://doi.org/10.16984/saufenbilder.659782
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http://www.saujs.sakarya.edu.tr/en/issue/52472/659782

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 Sakarya University Journal of Science 24(3), 521-530, 2020

Examination of Wear and Rockwell-C adhesion Properties of Nitronic 50 Steel

Coated with Pack Boriding Method

Ersan MERTGENÇ*1

Abstract

The Nitronic 50 steel is a nitrogen containing stainless steel, which has a high corrosion
resistance, and high strength but its surface resistance against wear is low, making it extremely
limited to use in areas subject to wear. In this study, in order to improve the material surface
and to investigate its effect on tribological properties, boronizing process was carried out by
used pack boriding method at 850 ° C, 900 ° C and 950 ° C for 4 hours. As a result of coating
process, the boride layer has a smooth and flat structure in SEM investigations, the coating
thickness varies between 9 µm and 36 µm and the boride layer thickness increases with
increasing temperature. While the hardness of the uncoated material was around 250 HV0.05,
the surface hardness of the material reached up to 1.712 HV0.05 with the coating process and
increased about 7 times. According to XRD analysis, the surface of the coating layer consisted
of phases FeB, CrB, Ni3B, Fe2B, Cr2B and MnB. Wear behavior was performed by ball-on-disk
wear test in dry environment. The friction coefficient and wear rate decreases with increasing
temperature, while the wear resistance is increased by 20 times compared to unboronized
sample. When the wear tracks were examined, the uncoated Nitronic 50 had an adhesive wear
mechanism, on the other hand the boronized samples had an adhesive and abrasive wear
mechanism together. The Rockwell-C adhesion test was carried out under a load of 1.471 N
and the resulting surface damages were evaluated according to the quality map. Boronized steel
at 850 °C is defined as HF3 type, at 900 °C and 950 °C at boronized steel it is defined as HF4
type and adhesion is acceptable.

Keywords: Nitronic 50, pack boriding, Rocwell-C adhesion, wear

1. INTRODUCTION ductility, toughness, work hardening capacity,

erosion and corrosion resistance increases [3-5].
Nitronic steels are seen as an erosion resistant
alternative to 13/4 martensitic stainless steel Nitronic 50 is a high nitrogen, weldable stainless
currently used [1]. Nitronic steels are mainly steel and superior to SAE 304 and 316 and 316L
austenitic stainless steels containing nitrogen as in strength and corrosion resistance [6] and is also
an alloying element in the matrix [2]. By adding known as 22-13-5 stainless steel [7]. They have
nitrogen to the content of stainless steels; strength, almost two times higher yield strength and good
corrosion resistance than standard 316 L stainless
steel [8], which is due to the high content of

*
Corresponding Author: ersanmertgenc@hotmail.com
1
Department of Railway Systems, Afyon Vocational High School, Afyon Kocatepe University, Afyonkarahisar,
Turkey. ORCID: 0000-0001-8247-2922
 Ersan MERTGENÇ
Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

chromium and molybdenum in the content, thus 2. MATERIALS AND METHODS

rivaling nickel alloys in seawater. Unlike most
austenitic stainless steels, they are not magnetic Nitronic 50 stainless steel was used in this study.
when working in cold or sub-zero temperatures The chemical composition is given in Table 1.
[7]. Nitronic 50 exhibits good mechanical
properties at low and high temperatures where
corrosion resistance and strength are required to Table 1. Chemical composition of Nitronic 50
be combined and is used extensively in a variety steel (wt. %)
of applications such as naval construction, pumps,
C Si Mn P S N Cr Mo Ni V
fittings, cables and heat exchangers [9].
0.032 0.6 5.04 0.027 0.0005 0.30 21.49 2.17 12.06 0.16

Although stainless steels exhibit high corrosion

resistance, low surface hardness is a major
disadvantage, especially when exposed to wear, The test samples were cut into ∅16 × 8 mm
and it is important to improve the tribological and dimensions and ground up to 1200 grid and
mechanical properties of their surfaces. In recent polished using diamond solution. Samples were
years, researchers have been working extensively placed in a stainless-steel box with Ekabor-II
on various coating techniques such as Pysical commercial powder. Then, they were boronized
Vapor Deposition (PVD) [10-12], Diamond-like in a temperature controlled chamber type furnace
Carbon (DLC) [13-17], Plasma Nitriding [18-20], under atmospheric pressure for 4 hours 850 °C,
Boronizing [21-23] to increase surface hardness 900 °C and 950 °C. After the completion of
through surface modification. boriding process, test specimens removed from
the sealed box were eventually allowed to cool
Fundamentally boronizing is a thermo-chemical down in still air.
process [24] diffusing the boron atoms from the
surface of materials by means of solid, liquid and For microstructure analysis, samples were cut
gas [25]. Boronizing can be carried out in solid, along longitudinal section, sanded with SiC
liquid and gas environments. Boron method is abrasive paper up to 120 - 1200 grit, polished with
widely used because of its low cost and simple. 1 µm alumina suspension and etched with
[26]. Pack boronizing is carried out in the stainless steel etch (HCl: HNO3: H2O to 1: 1: 1).
temperature range of 700 °C - 1000 °C for 0,5 to Coating layer, matrix microstructure, wear tracks
10 hours [27]. and boride thickness measurements were
examined by using a Leo 1430VP scanning
When the studies on Nitronic 50 stainless steel are electron microscope (SEM). The presence of
examined; It has been observed that mainly the boride in the coating layer was confirmed by x-
corrosion properties of the material have been ray diffraction (Shimadzu XRD-6000) using
studied. It is noteworthy that different methods CuKα (λ = 1.5406 Å) radiation at 20˚ - 90˚.
have been used for coating, but the effects of pack
boring on the material have not been investigated. Shimadzu HMV-2 micro-hardness tester was
used for hardness measurements. The
In this study, by using pack boriding method, measurements were made under conditions of 50
Nitronic 50 steel was treated at 850 °C, 900 °C g load for 10 seconds from the cross-sectional
and 950 °C temperatures for 4 hours, the surfaces of the coated samples to the matrix.
acceptability of the coating was evaluated by
Rockwell-C adhesion test and the effect of The wear tests of Nitronic 50 stainless steel coated
coating on the wear behavior was investigated. by pack boring method were carried out in the ball
disk system ball-on-disc system, dry conditions at
room temperature, under 5 N load, 0.3 m / s wear
rate and 500 m distance. 8 mm diameter WC-Co
balls were used in the wear tests. The surface of

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Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

each sample was cleaned with alcohol before and

after the abrasion wear tests. After the tests, the
wear volumes of the samples were quantified by
multiplying cross-sectional area by the width of
wear track obtained from a Tribotechnic
Rugosimeter. The wear rate was calculated with
the following formula.

Wear rate = Wear volume / (Applied load ×

Sliding distance), mm3 / Nm.

The Rockwell-C adhesion test was developed in

Germany and standardized in VDI 3198. The
Rockwell-C adhesion test, also known as the
quality test for coated compounds, is applied at a
load of up to 1471 N. It is mapped between HF1
and HF6 according to the condition of damage to
the coating in figure 1 [28]. According to this test,
which is easy to apply and evaluated especially
during quality control processes during
production; HF1-HF4 describes adequate
adhesion, ie the acceptability of the coating,
whereas HF5 and HF6 represent insufficient
adhesion [29,30].

Figure 2. SEM cross-sectional views of boronized

Nitronic 50 steel for 4 hours at a) 850 °C, b) 900 °C
Figure 1. Principle of the VDI 3198 indentation test c) 950 °C
[28]
Boride layer has a flat and smooth structure and
increase in boride layer thickness with increasing
temperature [31, 32].
3. RESULTS AND DISCUSSIONS
In steels, the thickness of the boride layer is
3.1. Characterization of Coating Layer and strongly influenced by the alloying elements as a
Thickness chorium, nickel and carbon in the substrate
material [33]. Especially the presence of
chromium makes it difficult to diffuse boron
The microstructures of Nitronic 50 steel from the atoms due to its lower solubility compared to iron
cross section of 850 °C, 900 °C and 950 °C for 4 and prevents the growth of iron borides [34, 35].
hours are shown in figure 2. The presence of as high as about 21 % chromium
in Nitronic 50 steel results in a reduced boride
layer thickness compared to steels. boride layer
thickness was given table 2 and measured at

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Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

850 °C 13 µm, 900 °C 29 µm and 950 °C 36 µm. According to xrd analysis, FeB, CrB, Ni3B, Fe2B,
It is observed that an increase in the boride layer Cr2B and MnB phases were formed on the surface
thickness is caused by the change in the process of the material depending on the process
temperature for a treatment time of 4 h. This is temperature. FeB and CrB phases increase with
due to the fact that the substrate material has high increasing temperature in boronizing treatment.
alloying elements, especially chromium and The reason for this is that the diffusion process is
nickel. accelerated with increasing temperature and the
layer thickness increases. Due to the high amount
of alloying elements such as Mn, Mo, Cr and Ni
in Nitronic 50 steel, different phases were
obtained due to these elements. The
microstructure and the mechanical properties of
the boronized material depend largely on the
chemical composition of the material, the
boriding temperature and the boriding time [38].
It is the reason why chromium based phases settle
in dominant peaks due to the chemical
composition of the material. On the other hand,
the presence of FeB phase as the dominant peak
Figure 3. Zones of the coating layer of boronized in iron-based peaks is close to the surface, while
Nitronic-50 steel for 950 ° C and 4 hours Fe2B phase settles between FeB phase and matrix
[35, 39, 40]. The coexistence of the CrB and FeB
When the figure 3 is examined, it is seen that there peaks is due to the fact that these phases are very
are 3 zones in coated Nitronic 50 steel; zone 1: difficult to distinguish due to their similar
coating layer FeB/CrB and composed of rich Fe, structure [41].
B, Cr, Ni alloys, zone 2: diffusion zone with
higher hardness than matrix but lower hardness 3.3. Hardness of Boride Layer
than boride layer, zone 3: steel matrix free of
boron [36, 37]. Micro-hardness measurements were performed
from cross-sectional area from surface to matrix
3.2. X-Ray Diffraction Analysis
(figure 5).

Figure 4 shows the x-ray diffraction analysis of

boronized Nitronic 50 steel at 850 °C, 900 °C and
950 °C for 4 hours.

Figure 5. Micro-hardness profiles of boronized

samples at 850 °C, 900 °C and 950 °C for 4 h.

The hardness of boronized Nitronic 50 steel was

Figure 4. X-ray diffraction patterns of boronized between 1080 HV0.05 and 1.712 HV0.05, while the
Nitronic 50 steel for 4 hours at a) 850 °C, b) 900 °C hardness of untreated steel was found to be (<)
c) 950 °C. 247 HV0.05. Hardness of boronized Nitronic 50

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Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

steel increased by seven times compared to the

hardness of non-treated Nitronic 50 steel.

3.4. Wear Properties

In Table 2, coating thickness, friction coefficient

and wear rate values of non-boronized and
boronized samples are given.

Table 2. Friction coefficient and wear rates of

boronized Nitronic 50 steel.
Conditions
Uncoated 850 °C – 4 h 900 °C – 4 h 950 °C – 4 h
Coating layer - 13 29 36
Friction coefficient 0.71 0.64 0.63 0.61
Wear rate x 10-8 (mm3 / Nm) 81.15 10,85 5.42 3,43

When the wear test results of Nitronic 50 steel

were examined, it was found that the friction
coefficient was 0.71 in the non-boronized sample,
whereas the friction coefficient in the boronized
samples at different temperatures for 4 hours
ranged from 0.64 to 0.61. Wear rate was 81.15
mm3 / Nm in non-boronized sample and lower
values were obtained in boronized samples. The
lowest wear rate was measured as 3.43 mm3 / Nm
in boron-treated sample at 950 °C for 4 hours.

When the wear tests of steels are examined in the

literature, the coefficient of friction changes
between 0.5 – 0.7 [42, 43, 44] and this shows that
this study is consistent with the literature. On the
other hand, surface investigators such as Kovaci
et al. [16], Cuao-Moreu et al. [45], Teng et al. [46]
and He et al. [47] have studied the tribological
properties of metal specimens by coating different
metal surfaces with different materials,
temperature, time and method. The reason for the
serious decrease in wear rate is the wear resistance
of the hard coating layer on the surface of the
material [48-50]. As seen from the XRD analysis,
the amount of high hardness phases such as FeB
and CrB increased.
Figure 6. Wear traces of boronized Nitronic 50 steel
The SEM images of the wear marks on the ball on
a) non-boronized, b) 850 °C – 4 h, c) 900 °C – 4 h,
disk system, against WC-Co balls, at 5 N load, d) 950 °C – 4 h
0.3m / s wear rate and 500 m distance are given in
figure 6. Wear traces vary according to boride layer
thickness [33, 51, 52]. When the surface
morphology of the wear marks is examined,
adhesive wear is seen in the non-boronized

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Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

sample, while abrasive wear is seen in both the boring at 850 °C (figure 7 (a)) and it is compatible
adhesive and abrasive wear by boring samples with HF3 according to the quality map. In
repeatedly cutting the coating surface by friction samples boronized at 900 °C (figure 7 (b)) and
pairs. The width of the wear tracks ranges from 950 °C (figure 7 (c)), delamination occurs along
1.400 µm to 320 µm and when the tracks are with radial cracks around the indentation craters
examined, it is seen that the largest wear tracks and the amount of delemination increases with
and damages such as smearing (plastic increasing boronizing temperature. This is due to
deformation) in the wear direction are non- the increase at the process temperature and the
boronized specimen (figure 6 (a)) and the depth of the hard and brittle structure FeB phase.
narrowest wear tracks are boronized at 950 °C However, the images of samples according to the
(figure 6 (d)), the highest temperature used for 4 quality test were identified as HF4 and represent
hours in the experiment. With the reduction of sufficient adhesion.
boride layer thickness, wear marks become more
deeper [53]. 4. CONCLUSIONS

3.5. Rockwell-C Adhesion The results obtained from the investigation of

tribological properties by coating the Nitronic 50
SEM images obtained from the adhesion test steel with pack boriding method at 850 °C, 900 °C
using a standard Rockwell-C hardness tester are and 950 °C for 4 hours are given below;
shown in figure 7. Damage to the boride layer and
adhesion strength are defined according to quality • The coating and the matrix interface
maps. According to the quality map, HF1-HF6 is exhibit a flat structure, which can be clearly seen
grouped between HF1-HF4 and HF5 and HF6 are the SEM observations. Boride layer thickness
defined as inadequate adhesion [28]. increased with temperature increase and reached
13 µm, 29 µm and 35 µm respectively.

• FeB, CrB, Ni3B, Fe2B, Cr2B and MnB

phases were formed in all boriding conditions and
FeB, CrB phases increased with increasing
temperature.

• The matrix hardness is around 250 HV0.05,

while the hardness of the boride layer ranges from
1080 HV0.05 to 1712 HV0.05, and the surface
hardness of the Nitronic 50 steel has increased
about 7 times.

• The friction coefficient and wear rate of

Nitronic 50 steel boronized by pack boring
method decreased with increasing boriding
temperature. While wear rate was 81.15 mm3 /
Nm for unborided sample, with boriding
treatment decreased to 3.43 mm3 / Nm and the
wear resistance of the material surface increased
Figure 7. SEM micrographs and radial cracks of VDI about 20 times.
adhesion test on boronized Nitronic 50 steel for
4 hours at a) 850 °C, b) 900 °C c) 950 °C. • As a result of the wear tests, non-boron
steel has been exposed to intensive adhesive wear
When the damage images of boronized Nitronic along with deleminations. In boronized samples,
50 steel are examined for 4 hours, it is observed
that radial cracks occur around the craters in the

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Examination of Wear and Rockwell-C Adhesion Properties of Nitronic 50 Steel Coated with Pack Boriding...

adhesive and abrasive wear types are seen stainless steel,” Wear, vol. 267, pp. 99-103,
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