Accepted Manuscript

Experimental studies of laser borided low alloy steel and

optimization of parameters using response surface methodology

S. Sashank, P. Dinesh Babu, P. Marimuthu

PII: S0257-8972(19)30181-1
DOI: https://doi.org/10.1016/j.surfcoat.2019.02.036
Reference: SCT 24353
To appear in: Surface & Coatings Technology
Received date: 4 October 2018
Revised date: 8 February 2019
Accepted date: 12 February 2019

Please cite this article as: S. Sashank, P.D. Babu and P. Marimuthu, Experimental studies
of laser borided low alloy steel and optimization of parameters using response surface
methodology, Surface & Coatings Technology, https://doi.org/10.1016/
j.surfcoat.2019.02.036

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 ACCEPTED MANUSCRIPT

Experimental studies of laser borided low alloy steel and optimization of

parameters using response surface methodology

S. Sashank1, P. Dinesh Babu*1, P. Marimuthu1

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School of Mechanical Engineering, SASTRA Deemed University, Thanjavur-613401,
Tamilnadu, India.

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*Corresponding Author

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P. Dinesh Babu

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Senior Assistant Professor, School of Mechanical Engineering
SASTRA Deemed University

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Thanjavur
Tamilnadu, India
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Email:dineshbabu@mech.sastra.edu, pdineshbabu81@gmail.com

Abstract
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Laser boriding technique was used to form boride layers on EN25 steel. The main aim of this
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current study is to form the hard laser borided layer on the low alloy steel surface and analyze the
effect of process parameters on borided layer hardness, depth, and width. The properties and
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microstructure (micro-hardness, boride layer width, and depth) are analyzed after laser boriding
process with different laser process parameters (power and speed). The micro-hardness of the
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boride layer was measured using the Vickers micro-hardness tester. The boride depth and width
was measured and captured using a machine vision inspection system. The existence of borides
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formed in the laser treated layer was confirmed via X-ray diffraction technique. The corrosion
rates of the laser borided and as received samples are observed in 3% NaCl solution using
Potentiodynamic polarization test. The response surface methodology was used to analyze the
effects of power, travel speed on the hardness and the boron layer width and depth. The two-
factor three-level full factorial design available in response surface methodology was used to
develop the regression model for laser boriding process. A multiobjective optimization technique
was used to optimize the laser process parameters to maximize the boron layer width and to
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minimize the boride layer depth. The validation trail assures that the expected value has good
conformant with the actual experimental value.

Keywords: laser boriding, response surface methodology, corrosion, micro-hardness,

optimization

1. Introduction
The high strength low alloy steels are designed to offer better mechanical properties (high

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strength and toughness) than normal carbon steels. The low alloy steel is normally supplied in

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quenched, tempered condition and used in automobile and aerospace industries. However,

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surface processing is required for this material to enhance the wear and corrosion resistance in
some critical applications [1,2].

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One of the competent thermo-chemical techniques of enhancing the hardness of steel materials is
by boronizing, which enriches the steel surface with boron by diffusion of boron atoms into the
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steel surface at high temperatures [3, 4]. Comparing with other usual thermo-chemical surface
modification techniques like carburizing and nitriding, the boronizing results in a much higher
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hardness, wear resistance, and corrosion resistance. Diffusion of boron into the metal surface and
alloys forms Iron borides, such as FeB and Fe2B needle-like phases depends on processing
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temperature, the chemical composition of the base materials. This boride formation significantly
enhances the corrosion resistance of iron-based materials and also tending to high hardness (up
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to 2000 HV), high abrasive wear resistance, high heat resistance even at elevated temperatures
[5].
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On the other hand, the major drawback of these boride layers is their high brittleness [5]. It is due
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to the high hardness of borides and by a huge hardness gradient between the boron zone and the
base material [5]. The brittleness of the borided layer can be minimized with the help of the
following methods. The single phase Fe2B layer formation [5] leads to lower hardness and which
reduces a hardness slope between the boride layer and the base material. The same can be
achieved by the formation of multi-component and complex borided layers [6-8]. The laser
surface treatment after diffusion boriding also shows a positive effect [9].

Now a day, the usage of laser increased drastically in surface engineering. The laser boriding is
one of the alternatives for diffusion boronizing process to minimize the brittleness of the borided
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layer. Laser boriding has two different processing methods. In the first method, the laser beam
re-melts the base material coated by boron paste [10]. In the second method, the alloying powder
with boron was introduced to the re-melting zone [11]. These two methods of laser boriding
enhance the mechanical properties and often overcome the drawbacks of diffusion boriding
process.

Morimoto et al.[10] examined the effect of laser boronizing of S45C steel. They mixed B2O3

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powder and Fe-B powder mechanically, and the mixed paste was applied on the substrate to form

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0.3 to 0.6 mm thickness. A 500W direct diode laser system was to heat the paste region. Their

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results revealed that the laser borided layer consisted of FeB and Fe2B with the thickness ranging
from 200-300 mm. Daria et al. [12] analyzed the effect of laser boronizing of Austenitic 316L
steel using a CO2 laser. Boron paste was coated on the specimen surface for 200 to 230 µm and

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melted by the laser beam power of 1.82kW and scanning speed of 2.88m/min. In the re-heated
zone, they observed a microstructure, composed of hard borides phases and a soft austenitic
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matrix with enhanced wear resistance and hardness.
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Hongyu et al. [13] boronized the 65Mn steel using powder boronizing agent in which ferroboron
and boron carbide as the boron source and potassium fluoborate as the activator. The boronizing
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temperature was 850 °C and the soaking time was 6 hours. The corrosion behavior of after
boronizing treatment was analyzed by in two acid mediums (hydrochloric solution and the weak
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acidic that fertilizer-containing soil). They observed a remarkable improvement in the corrosion
resistance of boronized steels. Simsek et al. [14] investigated the Corrosion behavior of pack
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boronized AISI 1050 steel in 10% H2SO4 acidic media, and their results confirm the
improvement in the corrosion behavior after the boronizing process. Aneta et al. [15] analyzed
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that, the corrosion resistance of medium carbon steel (C45) and high carbon steel (CT90) after
the diffusion boronizing and followed by laser (CO2)re-melting with a constant power of 1040W.
The diffusion boronizing was performed at 900 °C for 5 h. The boronized layer consists of iron
borides with micro-hardness ranged from 1400 to 1800 HV. Laser re-melting resulted with a
micro-hardness range from 1100 to 1700 HV. They observed that the laser boronized regions
were observed with enhanced corrosion resistance than the substrate.

Grum and slabe [16] evaluated the hardness and microstructure of laser surface treated 12 Ni
maraging steel. They laser surfaced the steel with a layer of Ni-Co-Mo alloy using a CO2 laser.
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Their analysis revealed diverse microstructure through the depth of laser surface specimens and
observed the through-depth microhardness variation in the heat-affected zone. Dorota et al. [17]
analyzed the influence of diffusion boriding and laser boriding on microstructure, micro-
hardness and corrosion resistance of Hardox 450 steel. They performed diffusion boriding at 950
°C for 4 h and for laser boriding they used amorphous boron paste, it is applied on the specimen
surface for a thickness of about 40 µm before laser heating. They conclude that the laser borided
samples characterized by resistance to corrosion then the diffusion borided samples.

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In addition to that, the laser material processing with appropriate input laser parameters forms

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the consistent fine-grained microstructure without pores [18]. Arguelles et al. [19] used central
composite design available in response surface methodology (RSM) to optimize the hardness of
the boron diffusion layer on Haynes alloy by considering two factors (temperature and time).

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The boronizing process was performed by commercial Durborid boron paste. The experimental
output values are evaluated by the analysis of variance (ANOVA). Their regression model shows
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that temperature has a significant effect, while time has no significant effect on the hardness.
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2. Experimental Procedure
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Even though several studies are attempting the laser boriding using different conditions, none of
them used RSM to investigate the optimal conditions for laser boriding process. RSM is an
experimental procedure, which allows a finding of the optimal conditions of a process in an
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experimental region selected. RSM reduces the number of experiments and helps in
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interpretation by making feasible the analysis for many factors and outlining their possible
mutual interactions [20, 21]. In this work, the influence of laser parameter (power and speed) on
boride layer hardness, width and depth were analyzed, and the regression model is developed
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using RSM, and optimum parameters are obtained using numerical optimization technique
(desirability approach of DOE). Boride layer was formed based on the optimum laser parameters
obtained, and corrosion resistance of EN25 steel samples was studied.
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2.1.Materials:

In this work, low alloy EN25 steel supplied in hardened and tempered condition was used as
base material. The chemical elements of this steel material were determined using a spectrometer
and were shown in Table 1 along with mechanical properties. The dimensions of the steel
specimens are 50 mm length, 40 mm width and 10 mm thickness.
The amorphous boron or iron-boron paste (particle size of about 50 μm) mixed with diluted

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polyvinyl alcohol solution was used as the coating material for laser boronizing process.

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Table 1 Chemical composition and mechanical properties of substrate material

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Chemical Composition [wt %]
C Si Mn Ni Cr Mo P S Fe

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0.35 0.30 0.59 2.80 0.63 0.55 0.02 0.02 Balance
Mechanical Properties
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Tensile Strength (MPa) Yield Strength (MPa) Hardness (HB) Elongation (%)
1000-1150 720-885 310-382 7-10
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2.2. Laser boronizing

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The top surface of low alloy steel substrate was coated with boron paste blended with a diluted
polyvinyl alcohol solution. The thickness of the boron paste was about 250 μm. An elcometer
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scale (range 25 to 3000 μm) was used to ensure the uniformity of the boron paste thickness
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applied over the substrate. Then the boron-coated surface was irradiated with carbon dioxide
laser beam of 4 mm diameter (focal length of 125 mm) and to prevent oxidation the argon
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shielding gas was supplied. The experimental trials were repeated for three times, and average
values were used for analysis. The schematic of laser boriding arrangement is shown in Fig. 1.
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Fig. 1. Schematic of Laser boronizing setup
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Fig. 2 shows the block diagram of the experimental system which contains laser boriding inputs
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and responses obtained. The major inputs for the laser boriding treatment are steel specimens,
amorphous boron paste, experimental design, laser process parameters and the outputs measured
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from the process are micro-hardness (borided zone, HAZ, substrate), boron layer thickness,
microstructure, and optimum process parameters.
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Fig.2 Block diagram of the experimental system

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2.3 Response Surface Methodology

Response surface methodology (RSM) consists of statistical methods, very much useful for
analyzing the effect of input parameters on responses (output) and it will generate the regression
equation. This regression model shall show the relationship between the input and output
parameters. The significance of the developed model can be analyzed by analysis of variance
(ANOVA) technique [22]. Two-factor three-level full factorial design available in design expert
software is used in this work. This design considered three levels for each factor. The parameter

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window used for laser treatment is shown in Table 2. The suitable values for the two factors, i.e.

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laser power (A) and travel speed (B) were chosen based on the initial trails and previous works.

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Optimum parameters can be obtained using the regression model developed and which satisfies
the optimization criteria. The numerical optimization module available in the design expert

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software is used for parameter optimization.

Table 2 Process parameters and the experimental design levels

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Levels
Sl. No Factor Unit
-1 0 +1
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1 Laser Power (A) kW 1.5 2 2.5

2 Scanning Speed (B) mm/min 300 400 500
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3. Results and discussion

3.1 Microstructure and phase analysis

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After laser treatment, the cross sections of the borided samples are polished and etched using 3%
nital and picral solution. The microstructure was observed using a light microscope and scanning
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electron microscope. The boride depth and width was measured and captured using a machine
vision inspection system.
Fig. 3.shows the macrostructure captured in the cross-section of the laser boronized samples
using a vision inspection system. The macrostructure images are shown in Fig. 3(a-c) are the
samples laser boronized at 300mm/min travel speed of laser beam for different laser powers such
as 1.5 kW (Fig. 3a), 2 kW (Fig. 3b), and 2.5 kW (Fig. 3c). Three different regions (seen in Fig
3(a-c)) observed in the macro-structure of the laser boronized samples. The first layer from the
top surface is the boride region, just below that a heat affected region is noticed, and the
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remaining bulk represents the core base material region. For the lower power of 1 kW, the depth
and width of the boride region obtained was 0.54 mm and 2.38 mm respectively with the heat
affected zone depth with 0.8 mm. The boride region depth and width was 0.68 mm and 3.18
respectively with the heat affected zone depth of 1 mm for 2 kW power. For the higher power of
2.5 kW, the depth and width of the boride region obtained was about 0.9 mm and 3.36 mm
respectively with the heat affected zone depth of 1.2 mm.

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(a) 2.38 (b) 3.18

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1 0.54 1 0.68
2 2

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3 3

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1mm 1mm

(c) 3.36
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1 0.9
2
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3
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1mm
Fig.3. Macrostructure observed in the cross section of laser boronized samples for 300 mm/min
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travel speed (a) 1.5kW, (b) 2 kW and (c) 2.5 kW; 1 borided zone; 2 hardened region (HAZ); 3
substrate
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The macrostructure results confirm that the width and depth of boride region increases with the
laser power increases. The heat input variation for different laser power will result in different
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boride depth and width. The higher the power (2.5 kW), more heat input is generated on the
surface where the boride paste was applied, and this resulted in more depth and width for the
given travel speed. Similarly, when the travel speed increases to 400 mm/min and 500 mm /min,
the depth and width of the boride layer reduced due to the lower interaction of the laser beam
with the material surface. The macro results confirm the importance of power and the speed on
the boride layer depth and width.
The microstructures of the laser boronized samples are shown in Fig.4(a-d) using different
magnification. The variation between the microstructure of laser borided zone, HAZ, and the
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base metal were visible in Fig.4(a). The compact boride region consisted of a mixture of iron
borides and martensite [5, 10]. The difference in HAZ and the base metal microstructure are
visible in Fig.4(b). To reveal the microstructure in the HAZ and the base metal, the images at
higher magnification were presented (Fig.4(c-d)). The presence of needle-like martensite along
with the retained austenite in the form of white precipitates was characterized in Fig.4(c). The
base metal microstructure reveals (Fig.4d) the bainite structure.

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(a) (c)

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needles of martensite

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boride zone

HAZ

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150 µm 25 µm

(b) (d)
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bainite
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HAZ
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BM
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75 µm 25 µm
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Fig.4. The microstructure of laser boronized EN25 steel (a) Three different zones, (b) HAZ and
base metal, (c) HAZ with martensite and retained austenite and (d) BM with bainite and ferrite.
HAZ-Heat affected zone, BM-Base metal.
During the laser melting of steel with boron, the instantaneous melting of boron paste (consists
of amorphous boron) and a fine layer of substrate (EN25 steel) formed a thin layer. As a result,
the formed layer has a different composition, properties, and microstructure than the substrate
and the coated boron paste [23]. Convection in the laser-heated molten pool was the significant
factor influencing the pool size and the microstructure of melted zone; this results in
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imperfections like porosity or variable penetration. Convection was also accountable for mixing,
hence affecting the composition of the laser melted zone [23].
The higher amount of iron borides formation close to the heated surface is due to its lower
density in contrast with the substrate. The lighter phase showed an ability to take up close to the
top surface, float due to the convection flows. The heat conduction and the rate of cooling were
enhanced in the occurrence of convection [24].The boron involved in the formation of iron
borides. In rapid cooling, the high carbon austenite regions relatively were transformed to

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martensite. Similarly, the cooling rate in the heat affected zone was also enough to form the

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martensite structure (Fig.4c). In addition to that, more amount of retained austenite was noticed

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in the HAZ region because of the high austenitizing temperature.

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Fig.5. XRD patterns of laser borided EN25 steel

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Laser-boriding processes on various steels were analyzed by the presence of iron borides with
martensite in the borided zone [5, 23]. Thus, the similar phases are expected in the present work.
The phase analysis was carried out after boriding in the laser treated region. The existence of
borides obtained in the laser treated layer was confirmed via X-ray diffraction (Shimadzu, Japan)
using CuKα with 5406Å radiation. XRD peaks (Fig.5) of the borided specimen ensured the
occurrence of three different iron borides (FeB, Fe2B, and Fe3B). The XRD peaks did not
provide data about the martensite phase presence. The martensite phase was identified in the
form of Feα. Likely, the proportion of the martensite phase in the microstructure was less.
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Nevertheless, taking the faster cooling rate in the laser process and the micro-hardness values
(1170-1315 HV0.5 in the laser melted region) into consideration, the presence of martensite was
assumed. Concurrently, the isolation of boron was taken place in laser melting process. As an
outcome, after re-solidification in few regions, iron richer phase Fe3B was identified. It was
ensured by the earlier research findings [5,23,25] which also states the formation of this phase
after boriding using a laser. In general, the carbon does not mix in FeB, and its solubility in Fe2B
is very less. Hence, in boriding carbon is traveled in the core direction by tracking the boron

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diffusion front and carbon is evicted from interstitial locations by boron, which creates borides of

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iron at the laser treated surface.

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3.2 Hardness analysis

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(a) LBZ AN (b) LBZ

HAZ HAZ
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BM BM
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(c)
LBZ
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HAZ
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BM

Fig.6. Micro-hardness profiles of laser borided layer in three different laser power and travel
speeds (a) 1.5 kW, (b) 2 kW and (c) 2.5 kW. LBZ-Laser borided zone, HAZ-Heat affected zone,
BM-Base metal.
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The hardness of the borided region was measured using the Vickers micro-hardness tester
(Shimadzu, Japan). The hardness test was performed under the constant load indentation of 5N
for the loading duration of 15 seconds. Fig.6 (a-c) shows the micro-hardness of EN25 steel
obtained after laser boronizing with different laser power and speed. In the laser borided zone,
the hardness observed for travel speeds (300-500 mm/min) was in the range of 1150-1210 HV0.5,
1168-1257 HV0.5 and 1215-1315 HV0.5 for 1.5 kW, 2kW and 2.5 kW laser power respectively. In
the heat affected zone, the hardness measured for travel speeds (300-500 mm/min) was in the

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range of 710-850 HV0.5, 774-880 HV0.5 and 812-925 HV0.5 for the laser power of 1.5 kW, 2kW

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and 2.5 kW respectively. Below that HAZ region, the base metal region was not affected by the

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laser heat and which retains the substrate hardness of 360 ±20 HV0.5.

The above hardness variation depended on the microstructural variation occurred due to laser

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boronizing process. The XRD results of the laser boronized specimens (seen in Fig.5) confirmed
the iron borides (FeB and Fe2B) present in the laser borided zone. The eutectic microstructure of
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iron borides and martensite formation in the laser borided zone is the reason for high hardness
(1170-1315 HV0.5). Then the micro-hardness along the depth decreased to 750-925 HV0.5 in the
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HAZ. This was caused by the microstructure of martensite and retained austenite obtained in the
HAZ. The next region below HAZ consisted of bainite microstructure, with the lower hardness
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of 340-380 HV0.5. The higher thickness of the heat affected zone diminished the hardness
gradient, and which resulted in a better bond of the boride layer with the substrate material. Also,
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it is more advantageous for stress distribution in laser borided layer and the base material.
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3.3 Corrosion resistance

The corrosion behavior was observed by potentiodynamic polarization method at the room
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temperature with the scanning rate of 0.5 mV/s using an electrochemical analyzer which
comprises cells with the working electrode of UNS S31803. The reference electrode was
saturated calomel while the counter electrode was set as platinum. Before the corrosion analysis,
the samples were ground and polished to the size of 10 mm2. Afterward, the samples were
cleaned catholically up to 8 minutes to eradicate out the oxide film and immersed into the 3.5%
NaCl solution for 180 minutes. The corroding potentials (Icorr) were recorded with a data-logger
for the total testing duration of 180 minutes.
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The corrosion samples are laser borided with the laser power 1.77kW and 500 mm/min laser
scanning speed. Corrosion resistance is dependent on the correctly chosen laser
processing parameters. The Potentiodynamic polarization curves are shown in Fig.7 represent the
corrosion resistance results of laser boronized and as received EN25 steel. In these curves, the
corrosion potential results observed is in the range from -1.5 V to 0.5 V are shown. In this study,
both the current and potential of corrosion were tested. In general, when the current value was
smaller, the resistance to corrosion was higher. From this study, it is concluded that the laser

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borided layer had a higher corrosion resistance than as received EN25 steel in NaCl solution.

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The iron borides (FeB, Fe2B, and Fe3B) formation in the laser treated surface area causes better
corrosion resistance. The laser boriding process left out more boron content in the melted zone
with less amount of iron. Besides, higher scanning speed (500 mm/min) caused less melting of

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the substrate and which reduces iron content in the melted zone. It is an added reason for better
corrosion resistance of borided layers formed using higher scanning speed. The more amount of
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boride eutectic microstructure left by the laser process was the reason for this property. The
increased amount of iron present in the unprocessed substrate affects the declining of the
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corrosion resistance [15].

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Laser borided
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Potential, V

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Base metal

Current, A/cm2
Fig.7. The potentiodynamic polarization of as received and laser borided EN25 steel
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(a) (b)
Cracks

Corrosion
products

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(c) AN (d)

Corrosion holes
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Fig.8. SEM examination of corroded samples surfaces (a,c) as-received and (b,d) laser boronized
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sample surfaces.

Fig. 8 shows the SEM morphologies of the corroded surface in the sodium chloride solution and
Fig. 8(a) and 8(c) represent the surfaces of the as-received sample’s SEM morphology after
corrosion and Fig. 8(b), and 8(d) shows the morphology of the laser boronized corroded sample
in different magnifications. Fig. 8(a) and 7(c) confirm that the surface of the as-received
corroded sample is distributed with more number of corrosion pits in large size and cracks,
which shows that the as-received sample has higher corrosion rate and it is mostly subject to
pitting type of corrosion. It is noticed from higher magnification shown in Fig. 8(c); corrosion
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holes are also formed in the as-received samples due to its inability to withstand the corrosion
resistance. It can be observed from Fig. 8(b) and 8(d) that, the surface of the laser boronized
sample is distributed with smaller corrosion pits, which confirms that the corrosion resistance of
laser boronized EN25 steel is enhanced as compared with the as received material and it is also
subjected to uniform corrosion.

3.4 Interaction Effect of Parameters

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Table 3 shows the responses (Hardness, boride width and depth) observed in the laser boronized

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samples at different laser process parameters (laser power and travel speed). Eleven experiments

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(seen in Table 3) were conducted as per the matrix arrived by 2-factor three-level full factorial
design.

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Table 3 Experimental input laser parameters and responses obtained after boronizing
Factor 1 Factor 2 Response 1 Response 2 Response 3
Std Run A: Power B: Speed Hardness Width Depth
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kW mm/min HV0.5 mm mm
1 3 1.50 300.00 1210 2.3821 0.5425
2 8 2.00 300.00 1286 3.1846 0.6850
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3 6 2.50 300.00 1315 3.3601 0.9175

4 11 1.50 400.00 1192 1.5235 0.4767
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5 2 2.00 400.00 1250 2.8681 0.5975

6 9 2.50 400.00 1283 2.9545 0.7586
7 10 1.50 500.00 1170 1.1864 0.3680
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8 4 2.00 500.00 1203 2.4245 0.4857

9 7 2.50 500.00 1250 2.6579 0.7111
10 5 2.00 400.00 1203 2.4245 0.4857
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11 1 2.00 400.00 1250 2.8681 0.5975

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The ANOVA statistics for Vickers hardness, boronized width and depth are shown in Table 4,
Table 5 and Table 6, respectively. They indicate that the regression model can be used to steer
the design space. In statistical analysis, a model with a higher F value (>1) and smaller p-value
(< 0. 05) is considered as significant [21]. The F values are 35.85, 37.23 and 46.13 for hardness,
width, and depth, respectively. The p values of all these models are < 0.05, which confirms the
significance of the models.

The values (R2 = 0.8896), (R2 = 0.9410) and (R2 = 0.9519) indicate that 88.96%, 94.1% and
95.19% of the variability in the results could be observed by the models of boride layer hardness,
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width, and depth, respectively. The observed R2 value closer to 1 showed good agreement
between the determined and obtained responses within the experimental range [26]. The adjusted
R2 (coefficient of determination) values are 0.8745, 0.9157 and 0.9312 for hardness, width, and
depth, respectively. These high values show the significance of these models. The predicted R²
values of hardness, width and depth are in reasonable agreement with the adjusted R² values,
with a difference less than 0.2. The adequate precision values are 18.393, 18.760 and 21.324 for
hardness, width, and depth, respectively. These values determine the signal to noise ratio, the

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values > 4 indicate that these models are desirable to the process.

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Table 4 ANOVA for Vickers hardness.

Sum of Mean p-
Source df F-value

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Squares Square value
Model 18586.67 2 9293.33 35.85 0.0001 Significant
A-Power 12696.00 1 12696.00 48.97 0.0001
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B-Speed 5890.67 1 5890.67 22.72 0.0014
Residual 2074.06 8 259.26
Lack of Fit 601.39 6 100.23 0.1361 0.9756 not significant
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Pure Error 1472.67 2 736.33

Cor Total 20660.73 10
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Std.Dev.:16.10, Mean: 1237.45, C.V.:1.30%, R2:0.8996, Adj.R2:0.8745, Pred.R2:0.8463

Adequate Precision: 18.3936.
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Table 5 ANOVA for boron layer width.

Sum of Mean
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Source df F-value p-value

Squares Square
Model 4.15 3 1.38 37.23 0.0001 significant
A-p 2.51 1 2.51 67.62 < 0.0001
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B-s 1.18 1 1.18 31.73 0.0008

A² 0.4582 1 0.4582 12.35 0.0098
Residual 0.2598 7 0.0371
Lack of Fit 0.1286 5 0.0257 0.3921 0.8276 not significant
Pure Error 0.1312 2 0.0656
Cor Total 4.41 10
Std.Dev.: 0.1927 Mean: 2.53, C.V.:7.61%, R2:0.9410, Adj.R2:0.9157, Pred.R2:0.8556
Adequate Precision: 18.7609
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The coefficient of variant (C.V.) determines the unexpected variability in the data. The observed
C.V. values are 1.30%, 7.61% and 6.80% for hardness, width, and depth, respectively. This low
C.V. foresees that these experiments have acceptable reliability and precision [27]. The lack of
fit (LOF) contrasts the pure error to the residual error from the duplicated experimental design
points. As the LOF values for hardness, width and depth are greater than 0.05, which indicates

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that the LOF of these models is insignificant [27]. The ANOVA test results from Table 4, Table

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5 and Table 6 shows that both the laser power (A) and travel speed (B) is to be the influencing

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parameters. The interactive (AB) effect and second order effects A2 and B2 are insignificant, and
they have not much influence on the hardness, width, and depth.

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Table 6 ANOVA for boron layer depth
Sum of Mean
Source df F-value p-value a
Squares Square
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Model 0.2322 3 0.0774 46.13 < 0.0001 significant
A-p 0.1667 1 0.1667 99.33 < 0.0001
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B-s 0.0561 1 0.0561 33.44 0.0007

A² 0.0094 1 0.0094 5.62 0.0496
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Residual 0.0117 7 0.0017

Lack of Fit 0.0034 5 0.0007 0.1638 0.9545 not significant
Pure Error 0.0083 2 0.0042
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Cor Total 0.2439 10

Std.Dev.: 0.0410 Mean: 0.6023, C.V.:6.80%, R2:0.9519, Adj.R2:0.9312, Pred.R2:0.9080
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Adequate Precision: 21.3242

The ANOVA statistical data (Table 4, Table 5 and Table 6) confirmed the significance of laser
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power. The p-values are 0.0001, 0.0001 and < 0.0001 for hardness, width, and depth,
respectively and which is less than the p-values stated for travel speed. Therefore, in this model,
the laser power is the most influencing parameter to control the responses.
The regression model in form of actual variables can be formulated by:
Hardness = +1178.7878+92.00P-0.31333S (1)

Width =-4.61907+7.85153P-0.004430S-1.63951P² (2)

Depth=+1.2310-0.607253P-0.000967S+0.235147P² (3)
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(a) (b)

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(c) (d)

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(e) (f)
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Fig.9. The interaction effect between laser power and beam travel speed on responses (a)
hardness contour plot (b) hardness surface plot, (c) width contour plot (d) width surface plot (e)
depth contour plot (f) depth surface plot.
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Fig.9 (e) and (f) represents the interaction effect of input parameters on boron layer depth in
contour and surface plot respectively. The surface plot indicates that increasing travel speed can
obviously reduce the boride depth.

The two-dimensional contour and three-dimensional surface graphs (seen in Fig. 9) are used to
display the interaction effect and behavior of outputs (hardness, width, and depth) for the
selected two input parameters. Fig. 9(a) and (b) showing the interaction effect of laser power and

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beam travel speed on boron layer hardness. The hardness can be maximized by increasing the

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laser power up to 2.5 kW. The interaction effect of laser power and beam travel speed on the

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boron layer width is represented by contour and surface plots in Fig. 9(c) and (d), respectively.
The response surface plot indicated that the travel speed is not much sensitive to the boride layer
width compared with power. With high laser power, the maximum of boride width can be

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3.5 Numerical optimization using desirability approach

Since there are many quadratic and interaction terms with independent parameters may not
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suitable to find the optimum laser process parameters. Thus, the combined objective optimization
technique should be used to solve this problem. The goal of multi-objective optimization is to
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find the conditions on the variables (independent) that pilot to optimal values of the output
variables. Here the aim is to determine the optimal combination of parameters that fulfill multi-
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objectives, to maximize the boron layer width and to minimize the boron layer depth.
Desirability function is a numerical approach to solve a combined objective optimization
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problem [28]. Desirable varies between 0 and 1.Desirability value 0, represent an unacceptable
design for the response selected, while the desirability value 1 represents the perfect
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configuration for the selected response.

Table 7 Criteria for optimization of parameters.

Process parameters Goal Lower limit Upper limit Importance

Laser power (kW) Minimize 1.5 2.5 5
Travel speed (mm/min) Maximize 300 500 5
Hardness (HV0.5) Is in range 1170 1315 3
Width (mm) maximize 1.18 3.36 5
Depth (mm) minimize 0.36 0.91 5
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Table 8 Optimum Solutions obtained as per design criteria.

Number Laser Power Travel Speed Hardness Width Depth Desirability

(kW) (mm/min) (HV0.5) (mm) (mm)
1 1.71 500.00 1179 1.7915 0.3961 0.821 (selected)
2 1.71 500.00 1180 1.8054 0.3973 0.821
3 1.74 500.00 1182 1.8570 0.4021 0.821
4 1.67 499.99 1182 1.8570 0.4021 0.820

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Fig.10 Contour plot of overall desirability for the laser boronizing condition
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The optimization criteria (goals and factor range) for this optimization model are listed in
Table 7. In the optimization process, all the parameters are given equal importance other than
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hardness, which is set in range. The optimal parameters should satisfy the objectives which are to
maximize the width and to minimize the depth. Table 8 shows the solutions obtained for the
given range and conditions. The contour plot for overall desirability is shown in Fig.10, which
presents the desirability for the laser boronizing conditions with a combined desirability value of
0. 821.
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Fig.10 and Table 8 show the optimal values. The optimal values of laser boronizing process
parameters are laser power 1.71kW and travel speed 500 mm/min. The optimized boron layer
depth and width are 0.3961 mm and1.7915 mm respectively.

Table 9 Validation test results.

Responses Predicted Desirability Experimental Error (%)

Hardness 1179 0.821 1199 1.66

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Depth 0.3961 0.821 0.4056 2.3

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Width 1.7915 0.821 1.8517 2.88

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The RSM approach is applied to plan the experiment. The values predicted by both responses
are obtained, and the optimization approach recommends the optimal process parameters. It is

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common to find the error between the actual and the predicted value after the execution of the
procedure.
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The predicted value is used to compare with the optimal parameters that are tested. The results of
validation tests and comparison are given in Table 9. The percentage of error between the actual
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value and the predicted value is less than 4.5%, which is in the acceptable range. The result
shows that the experimental values are in fine agreement with the predicted values. Therefore, it
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can be concluded that the optimal parameters obtained by response surface methodology can be
applied with high accuracy.
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4. Summary and Conclusion

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This study focuses on the formation of a borided layer on EN25 steel using laser boriding
process and developing the regression model for laser boronizing process. The interaction effects
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of process parameters are analyzed, and a multi-objective numerical optimization is performed to

obtain the optimum laser process parameters. The following conclusions are drawn from this
work:

1. The microstructure of borided steel consists of three zones: borided melted zone consists of
iron borides and martensite, heat affected zone (HAZ) with martensite microstructure and
substrate (bainite structure) without heat treatment. The eutectic microstructure formation
leads to high hardness (1170-1315 HV0.5) in the laser borided zone, and the martensite
structure in the HAZ resulted with 750-925 HV0.5. The higher thickness of the heat affected
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zone diminished the hardness gradient, and which resulted in a better bond of the boride layer
with the substrate material.
2. XRD patterns confirmed the formation of iron borides (FeB, Fe2B) in the boride region. The
separation of boron was taken place in laser melting process. As an outcome, after re-
solidification in few regions, iron richer phase Fe3B was also formed. The martensite phase
was identified in the form of Feα.
3. Corrosion results confirmed that the laser borided samples had a higher corrosion resistance

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than as received EN25 steel in 3%NaCl solution. The iron borides formation in the laser

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treated region enhances the corrosion resistance. The more amount of boride eutectic

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microstructure left by the laser process was the reason for this property. The SEM image of
the corroded surface of the laser boronized sample is distributed with smaller corrosion pits,

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which confirmed the corrosion resistance ability of laser boronized EN25 steel.
4. The RSM methodology has established the empirical models for micro-hardness, boron layer
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width, and depth. According to the regression models, the laser power has more influence on
the hardness and width and depth followed by travel speed. The optimal parameters including
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the laser power of 1.71kW, travel speed 500 mm/min lead to the predicted hardness, boron
layer width, and depth around 1179HV0.5, 1.791mm, 0.3961 mm, respectively.
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5. There is a reliable confirmation between predicted and actual results. The substantiation of
the regression models in predicting the responses is done by
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the proof experiment. It is determined that the error between the predicted results and the
experimental results is 1.66% for the hardness, 2.88% for the boride width and 2.3% for the
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boride depth.
6. It is concluded that RSM models are useful to find the optimum process parameters in turn to
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obtain the maximum boron layer width and minimum boron layer depth. These results are
more precise to control the laser boriding process parameters.

Acknowledgment
The authors gratefully acknowledge the laser facility provided by the Head, Magod laser Private
limited, Industrial Area Jigani, Bengaluru. The authors would like to thank Mr.Jagadish, Magod
laser, and for providing mechanical support to conduct the laser boronizing trails.
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Figure Captions
Fig. 1. Schematic of Laser boronizing setup
Fig.2 Block diagram of the experimental system
Fig.3. Macrostructure observed in the cross-section of laser boronized samples for 300 mm/min
travel speed (a) 1.5kW, (b) 2 kW and (c) 2.5 kW; 1 boride zone; 2 hardened region
(HAZ); 3 substrate
Fig.4. The microstructure of laser borided EN25 steel (a) Three different zones, (b) HAZ and

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base metal, (c) HAZ with martensite and retained austenite and (d) BM with bainite and

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ferrite. HAZ-Heat affected zone, BM-Base metal

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Fig.5. XRD patterns of laser borided EN25 steel.
Fig.6. Micro-hardness profiles of laser borided layer in three different laser power and travel

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speeds (a) 1.5 kW, (b) 2 kW and (c) 2.5 kW. LBZ-Laser borided zone, HAZ-Heat
affected zone, BM-Base metal.
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Fig.7. The Potentiodynamic polarization of as received and laser borided EN25 steel.
Fig.8. SEM examination of corroded samples surfaces (a,c) as-received and (b,d) laser boronized
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sample surfaces.
Fig.9. The interaction effect between laser power and travel speed on responses (a) hardness
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contour plot (b) hardness surface plot, (c) width contour plot (d) width surface plot (e)
depth contour plot (f) depth surface plot.
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Fig.10. Contour plot of overall desirability for the laser boronizing condition

Table Captions
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Table 1 Chemical composition and mechanical properties of substrate material

Table 2 Process variables and experimental design levels.
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Table 3 Experimental input laser parameters and responses obtained after boronizing
Table 4 ANOVA for Vickers hardness.
Table 5 ANOVA for boron layer width.
Table 6 ANOVA for boron layer depth.
Table 7 Criteria for optimization of parameters.
Table 8 Optimum solutions obtained as per design criteria.
Table 9 Validation test results.
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Highlights of this work

 It is the first attempt of laser boriding on EN25 (2.5% Ni Cr Mo steel) low alloy steel.

 The corrosion rates of the laser borided and as received samples are observed.

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 The response surface methodology was used to analyze the effects of parameters.

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 Optimum laser boriding parameters are identified using optimization technique.

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