JMDA-21-0224.R1 Proof Hi

Journal name
Influence of Heat Treatment on Microstructure, Mechanical

and Wear Properties of Maraging Steel Fabricated using
Direct Metal Laser Sintering (DMLS) Technique
Journal: Part L: Journal of Materials: Design and Applications
Manuscript ID JMDA-21-0224.R1
Manuscript Type: Special Issue: Advances in Metal Additive Manufacturing
Date Submitted by the

n/a
Author:
Complete List of Authors: S, Anand Kumar; Indian Institute of Technology Jammu, Department of
Mechanical Engineering; Indian Institute of Technology Jammu,
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Department of Mechanical Engineering
A, Sudarshan; intech additive
M, Snehith; intech additive
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P, Akshay; Indian Institute of Technology Jammu, Mechanical
Engineering
RVS, Prasad ; Intech additive
Yadav, SHUBHENDRA SINGH; Indian Institute of Technology Jammu,
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Mechanical Engineering
Materials Design, Materials Testing, Metallic Materials < Materials by

Keywords: Type, Plasticity < Materials: Mechanical Properties/ Strength, Metals
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Production < Materials Production
The present work investigates the influence of heat treatment on the

microstructure, mechanical and wear properties of direct metal laser
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sintering (DMLS) processed maraging steel. The microstructural

examinations were performed using optical microscopy, scanning
electron microscopy, energy-dispersive X-ray spectroscopy and X-ray
diffraction technique. The micro-hardness and tensile properties were
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determined using a micro-hardness tester and universal testing machine,

respectively. The unidirectional sliding wear test was performed using a
pin on disc wear testing machine for three different sliding velocities (0.8
m/s, 1.2 m/s and 1.6 m/s) and three different normal loads (5 N, 10N
and 15 N). The results showed that the heat-treated sample had finer
and non-continuous microstructure and harder intermetallic precipitate
Abstract:
phases, leading to higher hardness (~ 64 %) and higher tensile strength
properties (70-80 %) compared to the as-printed sample. The
unidirectional wear test results showed that the sliding velocity had a
significant effect on frictional and wear characteristics of DMLS processed
maraging steel. The wear resistance of the heat-treated sample was
three times higher than the as-printed sample, particularly at higher
sliding velocities. The lower coefficient of friction values (~ 24 %) was
observed for heat-treated sample compared to as-printed sample at
higher sliding velocities. The enhancement of wear performance and
tensile properties of the heat-treated samples are because of higher
hardness, harder intermetallic precipitate phase, refined microstructure
and lubricating oxide tribo-film.
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Journal name Page 2 of 35
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3 Influence of Heat Treatment on Microstructure, Mechanical and Wear Properties of
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5 Maraging Steel Fabricated using Direct Metal Laser Sintering (DMLS) Technique
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S. Anand Kumara*, Sudarshan Reddy Aniganib, Snehith Mathiasb, Akshay Pathaniaa,
8 Prasad Raghupatrunib, Shubhendra Singh Yadava
9 aDepartment
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of Mechanical Engineering, IIT-Jammu, Jammu-181221
11 bTechnology Development Cell, Intech-DMLS Pvt Ltd, Bangalore-560014
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13 *Corresponding author: [email protected]
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15 [email protected]
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Abstract
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23 The present work investigates the influence of heat treatment on the microstructure, mechanical
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25 and wear properties of direct metal laser sintering (DMLS) processed maraging steel. The
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27 microstructural examinations were performed using optical microscopy, scanning electron

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microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction technique. The micro-
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32 hardness and tensile properties were determined using a micro-hardness tester and universal
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34 testing machine, respectively. The unidirectional sliding wear test was performed using a pin on
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disc wear testing machine for three different sliding velocities (0.8 m/s, 1.2 m/s and 1.6 m/s) and
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39 three different normal loads (5 N, 10N and 15 N). The results showed that the heat-treated
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41 sample had finer and non-continuous microstructure and harder intermetallic precipitate phases,
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leading to higher hardness (~ 64 %) and higher tensile strength properties (70-80 %) compared to
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46 the as-printed sample. The unidirectional wear test results showed that the sliding velocity had a
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48 significant effect on frictional and wear characteristics of DMLS processed maraging steel. The
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50 wear resistance of the heat-treated sample was three times higher than the as-printed sample,
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53 particularly at higher sliding velocities. The lower coefficient of friction values (~ 24 %) was
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55 observed for heat-treated sample compared to as-printed sample at higher sliding velocities. The
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3 enhancement of wear performance and tensile properties of the heat-treated samples are because
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6 of higher hardness, harder intermetallic precipitate phase, refined microstructure and lubricating
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8 oxide tribo-film.
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11 Keywords: Heat treatment, Microstructure, Mechanical Properties, Wear Performance, Maraging
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steel, Direct Metal Laser Sintering Technique.
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17 Introduction
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20 The direct Metal Laser Sintering (DMLS) technique has been widely used to manufacture
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metallic materials and their alloys with superior mechanical properties compared to conventional
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25 manufacturing and powder metallurgy processing techniques [1-6]. DMLS offers a wide range of
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27 recompenses such as simplified product design approaches, complex geometries, reduction in

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29 weight because of lattice structures and reduction in material wastage [7-11]. In DMLS, the 3D
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32 CAD model is directly used to fabricate the final product via layer by layer method. Maraging
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34 steel is popularly known among various steel grades because of its improved tensile strength,
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moderate ductility, better weldability and machinability [12-13]. The use of maraging steel is
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predominantly found in two sectors (i) in the aerospace industry for its high strength, moderate
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41 ductility and weldability and (ii) in the tooling and die mould industry due to its good
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43 machinability [14]. The maraging steels differ from conventional steels since a metallurgical
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reaction is enough to harden them without carbon involvement, making it a particular steel class
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48 [15]. The recent studies demonstrate that the DMLS processed maraging steels with superior
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50 mechanical properties [16] and tribological performances [17] are obtained through better DMLS
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52 process planning and control. The maraging steels fabricated using the DMLS process differ
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55 significantly from the conventional processing route in terms of rapidly cooled microstructure
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3 with enhanced tensile properties under as-printed condition because of the high cooling rates
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6 during layer by layer processing [18].
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9 The extensive use of maraging steel in die and mould components during varying operating
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11 conditions leads to significant wear, which eventually deteriorates the die and mould components
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along with affecting surface qualities of the parts being processed and other frequent replacement
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16 and refurbishment of a die and mould materials are not economical [19]. Therefore, a necessity
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18 arises to fabricate die and mould components with superior tribological life in mechanical and
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metallurgical properties, targeted for tooling industries. In this regard, several researchers
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23 attempted to address the superior tribological performance of DMLS processed maraging steel.
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25 Tan et al. (2018) [20] investigated the effect of post-heat treatment to improve the wear
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27 resistance of DMLS-produced maraging steel. They reported a remarkable improvement in

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mechanical properties and a two-fold increase in wear resistance for heat-treated maraging steel.
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32 Further, Yin et al. (2018) [21] investigated the effect of optimized ageing treatment on DMLS
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34 processed maraging steel to bring out superior wear resistance and mechanical properties. They
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observed the degraded wear behaviour and mechanical properties under both lower and higher
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39 ageing treatment conditions than optimum intermediate ageing treatment. It appears that gaining
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41 required wear resistance and mechanical strength significantly depends on microstructural
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constituents such as grain size, harder phases, reinforcements in DMLS processed maraging
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46 steel. It is widely accepted that the tool and dies mould longevity not only affected by higher
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48 surface hardness. But, also another factor such as secondary harder phases as reinforcements. For
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50 instance, tungsten carbide (WC) is known to possess favorable properties, which helps increase
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53 tribological performance, especially under extreme operating circumstances such as elevated
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55 temperature and greater frictional resistance. Kang et al. (2018) [13] investigated WC reinforced
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3 maraging steel fabrication using DMLS. They reported five-fold enhancement in tribological
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6 performance of WC reinforced maraging steel compared to maraging steel without WC. They
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8 attributed the improvement to the microstructural changes because of the diffusion of W element
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10 through grain boundary. Yan et al. (2019) [22] attempted to compare two additive manufacturing
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methodologies such as cold spray and DMLS, to fabricate the maraging steel reinforced with
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15 WC. They reported that DMLS had higher wear resistance (about ten-fold) than the one
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17 processed via cold spray route due to better metallurgical bonding characteristics in DMLS
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processed samples than cold sprayed samples.
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23 It should be noted that the maraging steels are extensively employed in the cold-extrusion die
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25 and mould applications [23]. In the course of the cold-extrusion process, the dies or moulds are
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27 likely to get exposed to fluctuating loading situations and a range of sliding velocity of ram. As a
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result, worsening of the surface finish of the die or mould surfaces are expected. Further, the dies
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32 and mould’s service life would decrease drastically because of the dynamically changing contact
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34 pressure/stresses scenarios at the work material's interface being extruded and die or mould
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surface. Therefore, it is imperative to evaluate the tribological performance of die and mould
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39 components made from DMLS processed maraging steel. It appears that equally important to
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41 understand work materials' wear behaviour like metallic alloys and metal matrix composites.
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Therefore, investigation on the sliding velocity effect (similar to extrusion speed) is essential in
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47 view of designing die and moulds with higher service life and realizing low-cost extruded parts.
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49 Hence, understanding the effect of sliding velocity on the tribological performance of DMLS
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51 processed maraging steel is required and becomes the subject of interest.
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3 It should be noted that the research work carried so far on the tribological studies of maraging
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6 steel are focused on (i) the relative performance between as-printed and the ageing/heat-treated
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8 maraging steel samples fabricated using DMLS, (ii) comparison of processing methods (cold
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10 spray and DMLS) of WC reinforced maraging steel. Given increasing demand for maraging steel
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usage in the cold-extrusion die and mould applications, it is essential to understand the interplay
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15 between the die and mould fabricated out of DMLS processes and varying loading and range of
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17 sliding velocity (deformation speed) encountered. Because of the above, the present work
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investigates the influence of different sliding velocity and normal load independently and their
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22 combined effect on the unidirectional sliding wear behaviour of DMLS processed maraging steel
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24 under as-printed and heat-treated conditions. The above study's outcome would find the
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26 pathways to qualify the die or mould components suitable for producing high-quality and cost-
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29 effective metal formed end-products.
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32 In this present study, 18Ni-300 maraging steel has been fabricated by the DMLS technique.
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34 Further, the heat treatment process has been carried out to enhance the strength of DMLS
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processed maraging steel. The microstructural characterization of heat-treated and as-printed
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39 samples was performed using an optical microscope, scanning electron microscopy (SEM) and
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41 X-ray diffraction (XRD) techniques. The DMLS processed maraging steel under as-printed and
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heat-treated conditions were characterized for Vicker’s micro-hardness, tensile property
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46 examinations. The unidirectional sliding wear behaviour under different sliding velocities to
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48 simulate situation similar to the cold-extrusion process are attempted. Besides, the digital
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50 microscopy technique has been used to characterize the worn surface of samples.
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3 1. Experimental Details
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7 The powder characterization was performed using an SEM with Energy-Dispersive X-ray
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9 Spectroscopy (EDXS) attachment (Ultra55 FESEM, Oxford). The 18Ni-300 maraging steel
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11 powders used in the present was processed via a gas atomized route and had a spherical
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morphology ranging from 15 to 50 μm. The powder particles were found to be nearly spherical.
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16 However, a bimodal distribution was seen in the powder's morphology, as shown in Figure. 1
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18 and the powder has an average size of 30 μm.
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39 Fig.1: SEM images showing spherical morphology of powder particles
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Figure. 2 shows a considerable fraction of particles having splats on top of them, and there is no
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45 significant difference in the chemical composition between the spherical particles and the splats.
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47 The SEM-EDXS analysis to study the chemistry of maraging steel powder at 1 and 2 locations is
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shown in Table. 1 and it is observed that spherical particles and splats are almost the same.
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21 Fig.2: SEM-EDXS image showing the elemental composition of localized powder particle
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spherical and splat.
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27 Table. 1. Elemental composition of 18Ni (300) Maraging steel

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30 Element Powder (#1) Wt % Splat (#2) Wt %

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Al K 0.30 0.28
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Ti K 0.92 0.91
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34 Fe K 66.36 66.63
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36 Co K 9.49 10.77
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37 Ni K 18.31 16.34
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Mo L 4.62 5.08
40 Total 100 100
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46 The maraging steel powders were processed under the direct metal laser sintering route by
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48 maintaining the inert atmosphere using the EOSM-280 machine. The optimized DMLS process
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50 parameters are shown in Table. 2. Figure. 3 shows the scheme of the fabricated DMLS sample
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used in the present study. The DMLS processed samples were subjected to heat-treatment with a
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3 heating rate of 150° C/hr up to 460° C and holding for 6 hours and cooled to room temperature in
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6 the electrical furnace (Nabertherm furnace, INTECH).
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9 Table 2: DMLS process parameters
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13 DMLS process value
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16 parameters
Laser power (W) 260-300
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18 Scan speed (mm/sec) 850-1000
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Hatch distance (mm) 0.1-0.12
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23 Layer thickness (µm) 50
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25 Laser spot diameter (µm) 80
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44 Fig.3: Built direction (BD) of DMLS processed maraging steel: Transverse-T (X-BD);
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46 Longitudinal-L (Z-BD). DMLS processed maraging steel nomenclature used for the wear
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48 test.
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52 The microstructural investigations on the DMLS samples were performed using an optical
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54 microscope (Zeiss Axiacam) and SEM. The microstructure was obtained using an etchant (15 ml
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1
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3 water, 50 ml HCl, 20 ml acetic acid and 15 ml HNO3) via the swab etching method. The porosity
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6 of the DMLS fabricated samples were obtained using Image-J software. The X-ray diffraction
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8 analysis of raw powder and DMLS samples were obtained by employing an X-ray diffractometer
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10 (Miniflex, Rigaku) with Cu-Kα radiation. The micro-hardness of the DMLS processed samples
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was performed using Vicker’s micro-hardness tester (Shimadzu) with a load of 300 grams and a
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15 dwell time of 10 seconds. The indent was made on the sample's surface in three random places,
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17 and the average value has been reported. The tensile test was performed as per the dimension
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shown in Figure. 4 using a universal testing machine (TUE-C-Series) of 600 KN capacity, at a
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22 strain rate of 0.006 mm/sec.
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38 Fig. 4: Tensile test sample. All dimensions in mm.
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41 The unidirectional sliding wear behaviour of DMLS processed samples was analyzed using a pin
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43 on disc tribometer (TR-200 Ducom instruments). Before the wear tests, the samples were
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polished with emery paper and washed with acetone. The tests were carried out in dry
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48 conditions. The details of the wear test are given in Table 3. The test configuration employed in
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50 the present study was a cylinder on flat contact mode, as shown in Figure. 5. The Hertz theory
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[24] was employed to determine the initial maximum Hertzian contact pressure (P) and contact
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55 radius (a) using equations 1 and 2. Further, for a cylinder on flat contact configuration, the term
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1
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3 d2 in equation 2 tends to infinity [25]. The contact pressure and contact depth between tribo-pair
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6 are given in Table 4.
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9 2𝐹
10 𝑃𝑚𝑎𝑥 = ………………………………..(1)
𝜋𝑏𝑙
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14 1 ― 𝑣21 1 ― 𝑣22
15 2𝐹( + )
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𝐸1 𝐸2
𝑏= …………………(2)
17 1 1
18 𝜋𝑙( + )
19 𝑑1 𝑑2
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26 Table 3: Unidirectional sliding wear test parameters
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27 Test Parameters Descriptions

28 Test sample Diameter = 10 mm, Length = 10 mm
29 Hardness: As-printed = 390 HV0.3; Heat treated = 640 HV0.3
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Poisson’s ratio (v1) = 0.3
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32 Elastic modulus(E1) = 190 GPa
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34 Counter disc – Diameter – 165 mm
35 EN31 steel Hardness – 68 HRC
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Poisson’s ratio (v2) = 0.3

37 Elastic modulus(E2) = 215 GPa
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39 Normal load (N) 5, 10, 15
40 Sliding speed (m/s) 0.8, 1.2, 1.6
41 Test time (min) 30, 40, 60
42 Lubrication condition Dry
43 Temperature Room Temperature
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19 Fig. 5: Unidirectional sliding wear test configuration- a cylinder on flat contact mode
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Table 4: Hertz’s contact pressure and contact depth
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26 Load (N) Contact Pressure (MPa) Contact depth (mm)
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27 5 59.5 0.004
28 10 84.0 0.006
29 15 102.9 0.007
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35 The wear loss was quantified using a weighing balance (Shimadzu- ATX224) of each sample
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37 before and after the wear test. The three dimensional (3D) wear track morphology and line
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roughness of all the worn-out samples was performed by employing a digital microscope
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42 (Olympus-DTX520).
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45 3. Results and Discussion
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48 3.1. Optical Microscopy: Microstructural and Porosity Characterizations
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52 Figure. 6 illustrate the optical micrographs of as-printed and heat-treated samples in both
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54 longitudinal and transverse directions. The microstructure of both as-printed and heat-treated
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3 samples in longitudinal direction shows the melt pool average depth of about ~ 65 µm in Figures
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6 6 (a) and (b). Figures. 6 (c) and (d) represents the transverse direction microstructure of both as-
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8 printed and heat-treated samples, which shows the melt pool average width of about ~ 80 µm.
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10 The optical micrographs shown in Figure 7 show little or no porosity in all the samples. The
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density values were found to be above 99.9 %. Figure. 7e shows that the heat-treated sample had
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52 Fig.6: Optical microstructures of as-printed: (a) longitudinal direction and (c) transverse
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54 direction, heat-treated: (b) longitudinal direction, (d) transverse direction.
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49 Fig. 7: Optical micrographs showing porosity (a) as-printed: longitudinal direction, (b)
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heat-treated: longitudinal direction, (c) as-printed: transverse direction, (d) heat-treated:
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54 transverse direction,
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3 (e) Plot showing porosity variations of DMLS processed samples: L- longitudinal and T-
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9 3.2. SEM Microstructural Characterization
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12 Figures. 8 - 10 shows the scanning electron micrographs of DMLS fabricated samples. The
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longitudinal and transverse SEM images (Fig. 8 ‘a’ and ‘b’) of the as-printed sample expose the
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17 epitaxial growth of enormously refined cellular grains across the hatch overlap region [26]. Fine
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19 cellular structure during the DMLS process could be attributed to the high thermal gradients that
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result from the instant melting and solidification process [27]. Figures. 9 and 10 show the
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24 longitudinal and transverse SEM images of heat-treated samples, displaying the oxides formed in
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26 the matrix. These oxides enriched in Mo and Fe appear in a blister-like morphology after the heat
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28 treatment (Fig. 9b and 10b). Since the ageing heat treatment was performed at elevated
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31 temperature, the grain boundaries tend to disjoint, as shown in Figure. 10a.
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34 It is evident from the data that the ageing heat treatment at 490 °C for 6 h had led to an
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36 enhancement in hardness because of the presence of the precipitates of Ni(3) (Mo, Ti) and
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38 Fe(2)Mo intermetallics phases [21, 28]. The precipitates are shown in red-coloured arrows in
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Figure. 10a. The EDXS analysis correlates well with the agreement that the presence of
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43 intermetallic phases in the heat-treated sample.
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52 Fig.8: SEM images of as-printed samples: (a) longitudinal (b) transverse
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Fig.9: SEM images of heat-treated longitudinal direction of DMLS samples.
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45 Fig.10: SEM images of heat-treated DMLS samples in the transverse direction.
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48 3.3. X-ray Diffraction Characterization
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51 Figure. 11 represents the X-ray diffraction spectrum of raw powder, and DMLS processed
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54 samples. It is seen that the heat treatment affects the growth in the austenite phase. The
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56 martensite in the metastable state tends to convert into the austenite phase during the ageing
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3 treatment performed for longer times. The liberated Ni diffuses into the nearby Fe phase, which
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6 goes together with Ni3 (Mo, Ti) conversion to the much stable Fe2Mo precipitates upholds the
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8 austenite reversion [29]. Further, the Ni-rich zones create a quick austenite reversion potential
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10 [30].
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38 Fig. 11: XRD spectrum of raw powder and DMLS processed samples
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41 3.4. Mechanical Properties of DMLS Processed Samples
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45 3.4.1. Micro-hardness Evaluation
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48 Figure. 12 shows the micro-hardness of the DMLS processed samples in both longitudinal and
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50 transverse directions. The heat-treated sample showed a higher hardness value of 640 HV0.3
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(~ 64 %), while the as-printed sample had a hardness value of 390 HV0.3. Also, both directions'
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55 hardness values are almost the same, indicating that DMLS processed samples have a desirable
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3 characteristic of isotropic property, which is appropriate for most of the practical applications.
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6 The heat-treated (aged) sample shows the highest fraction of small-angle grain boundaries
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8 because of the development of enormous small precipitates and intermetallic phases, which
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10 hinders the dislocation movement resulting in the enhancement of hardness and mechanical
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properties. Various researchers had reported similar results [15, 16]. It is widely accepted from
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15 Archard’s law that the harder materials possess superior tribological performance for practical
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17 applications involving sliding contacts. Therefore, the hardness of the material plays a role major
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in deciding the tribological performance of the tribo-pair in various operating conditions.
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44 Fig.12: Micro-hardness values of DMLS processed maraging steel:
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L- longitudinal and T-transverse.
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3 3.4.2. Tensile Properties of DMLS Samples
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7 Figure. 13 shows the tensile properties of the DMLS processed samples in both longitudinal and
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9 transverse directions. It is generally agreed that the yield strength and ultimate tensile strength of
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11 the heat-treated sample are higher (70-80 %) compared to the as-printed sample. The
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enhancement in mechanical strength properties is attributed to precipitation hardening
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16 mechanism due to hard precipitate particles and intermetallic phases acting like an obstacle for
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18 dislocation motion during the plastic deformation process. Various researchers had reported
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similar results [20, 21]. Further, it is interesting to note a reasonable good relationship between
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23 hardness and tensile properties in the present study. The ultimate strength is approximately three
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25 times the micro-hardness values measured, which is in line with ASM handbook analysis on
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27 alloy steels [31]. Also, there is a noticeable drop of 60 % in elongation after heat treatment
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resulting in a ductility reduction compared to the as-printed sample. Further, there is no
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32 significant difference in tensile properties among longitudinal and transverse directions
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34 demonstrating isotropic behavior, which corroborates well with the micro-hardness value trend.
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21 Fig.13: Tensile properties of DMLS processed samples in different conditions:
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The fractographic images of the tensile tested DMLS sample are shown in Figure. 14 and 15.
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36 It is evident from the data that the significant presence of dimple morphologies and cracks are
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38 seen in Figure. 14. Since the as-printed sample fractured after considerable plastic deformation
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resulted in a ductile fracture. A trans-granular fracture mode is always observed in ductile
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43 fracture [32]. The metallic materials feel a large plastic deformation during the tensile test,
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45 leading to micro-cavities on the precipitates or on the imperfections, which eventually leads to
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47 the coalescence of micro-cavities fracture events. Figure.15 shows the presence of facets, which
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50 are the typical signature of brittle fracture phenomena [33]. The heat-treated sample due to
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52 precipitates' presence enhances the hardness and strength of a material, but the material's
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1
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3 ductility reduces, which causes the brittle fracture [34]. Similar results were reported by other
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6 researchers [20, 21].
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9 It further interesting to note that the two different particles were observed on the fracture surface
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11 of heat-treated samples, it appears that the balling defects generated in the DMLS process. It has
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13 been suggested that the balling defects do not affect the properties of DMLS processes materials
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[21]. The EDXS analysis shows that particle “P1” is resembling to starting virgin powder
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18 chemical composition, and the other particle “P2” had chemistry more closely matching with the
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40 Fig.14: SEM images of tensile fracture surfaces of the as-printed samples
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34 Fig.15: SEM images of tensile fracture surfaces of the heat-treated samples
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38 3.5. Tribological Behavior DMLS Processed Samples
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41 3.5.1. Influence of Sliding Velocity on Frictional Characteristics of DMLS Processed
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43 Sample
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47 Figure. 16 shows the influence of sliding velocity on the coefficient of friction (CoF) values at a
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49 normal load of 5 N. It is evident from the data that, during wear tests, the stable response in CoF
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51 values has arrived about 100 seconds at all sliding velocities. A similar trend was observed for
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samples tested under normal loads 10 N and 15 N. It is interesting to note that a significant
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56 reduction (~ 24 %) in friction in the case heat-treated sample observed as compared to
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1
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3 significantly less (~ 8 %) for the as-printed sample while the sliding velocity increment from 0.8
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6 m/s to 1.6 m/s. This indicates a substantial lessening of friction at tribo-pair interface while
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8 sliding against the heat-treated sample. The rise in temperature at the tribo-pair interface is due to
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10 frictional heat generated during sliding [35].
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Therefore, the rise in temperature at the contact interface facilitates the development of oxides.
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16 This oxide-based protective tribo-film are presumed to be the driving factor in reducing CoF
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18 values at higher sliding velocities for the heat-treated sample. Further, a similar observation has
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been made by Yin et al. [21] for DMLS heat-treated maraging steel. Further, CoF is the measure
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23 of resistance to the relative motion between materials under contact loading. Generally, the
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25 friction force developed during a wear test has two parts: adhesive and other is deformation [36].
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27 In the present work, the adhesive part is presumed to be operative since the steel to steel tribo-
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pair encountered in the present study. In general, the hardness values of contact materials during
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32 sliding event influences the actual contact area. For instance, soft materials will have more
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34 contact area due to the indenting nature of harder material, which can have an adverse effect on
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the CoF values during contact loading. Therefore, It is generally agreed that the as-printed
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39 sample being comparatively softer than the heat-treated sample, tend to have more actual contact
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41 area and tends to show up larger CoF values. It is widely accepted that the adhesive part's
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influence could be effectively controlled by enhancement of the hardness of the sample, which
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46 decreases the overall CoF values. Therefore, a heat-treated sample with ~ 64 % harder than the
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48 as-printed sample could minimize the adhesive part of the friction force resulting in less CoF
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50 values.
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45 Fig.16: Friction curves of as-printed and heat-treated samples
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3.5.2. Influence of Sliding Velocity on Wear Characteristics of DMLS Processed Sample
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52 Figure. 17 3D plot shows the effect of sliding velocities on the wear performance of the DMLS
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54 processed samples. It is evident from the data that the sliding velocity has a linear relation to the
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3 wear loss for DMLS processed samples. The heat-treated sample shows superior wear resistance
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6 compared to the as-printed sample under all sliding velocities and normal loads, especially at
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8 high sliding velocity and normal load. It is primarily due to higher hardness, larger tensile
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10 strength, and lubricating oxide protective layer.
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13 Further, it could be seen that at higher sliding velocity and normal load, there is a significant
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improvement of three times higher wear resistance for the heat-treated sample than the as-printed
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18 one. The increment of sliding velocity induces a larger plastic deformation magnitude, which
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20 further results in significant material loss during sliding [37]. Further, at the tribo-interface,
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locally, a high-temperature situation develops due to the high sliding velocity, which promotes
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25 thermal softening among tribo-pair, generating more wear debris in the case of the as-printed
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27 sample[38]. It is well established that the ageing heat treatment can induce the secondary harder
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29 phases and intermetallic reinforcement particles (such as μ, S and X), which significantly
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32 improve the mechanical properties [21, 39, 40]. It is clear from the Figures. 9 (d) and 10 (c) that,
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34 the heat-treated sample exhibits (because of the presence of the intermetallic phases) higher wear
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resistance under all sliding velocities. This suggests that intermetallic phases in the matrix of
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maraging steel have a remarkable effect on the superior tribological performance at larger sliding
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41 velocities. The improvement in the hardness and tensile strength with the intermetallic phases
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43 due to ageing heat treatment indeed offer a beneficial effect on frictional and tribological
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characteristics. Given the above, the enhancement of hardness and tensile strength because of
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48 ageing heat treatment is a dominant factor resulting in substantial improvement in wear
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50 resistance, which agrees with well-established Archard’s law.
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31 Fig. 17. 3D plot of wear resistance comparison: (a) as-printed and (b) heat-treated samples.
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34 The beneficial aspects of intermetallic phases towards enhancing the tribological performance of
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metallic materials have been well studied. Yin et al. [21] reported that the positive effect of
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39 ageing heat treatment on a maraging steel's tribological characteristics. The enhancement was
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41 attributed to precipitation hardening. In another study by Yao et al. [41], intermetallic phases
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were intentionally generated to harness the benefit of enhancing the mechanical and tribological
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46 performance of Stellite alloys embedded with molybdenum. Therefore, it is evident from the data
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48 that the intermetallic phases can be a promising hardening phase and the most appropriate
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50 alternative for carbides in maraging steel. It is generally agreed that the improvement in high-
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53 temperature frictional and tribological characteristics due to the presence of harder intermetallic
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55 phases has been reported in the case of ferrous based alloys. It is shown that the intermetallic
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3 phases have exorbitant properties such as hot-hardness, particularly at high sliding velocity and
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6 high loading conditions [42]. Hence, the presence of harder intermetallic phases to improve
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8 elevated-temperature wear resistance can shed light on critical engineering applications such as
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10 tool and dies suitable for hot metal forming processes.
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Figure. 18 shows the surface response coupled with contour plot for wear loss of both the DMLS
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16 processed samples. The trend is observed to be similar in both the DMLS processed samples.
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18 It appears that, the wear loss of the as-printed sample at a normal load of 10 N and all sliding
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velocities (800, 1200 and 1600 mm/s) is relatively higher than the heat-treated sample wear loss
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23 at a normal load of 15 N and all sliding velocities (800, 1200 and 1600 mm/s). It suggests that
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25 the heat-treated sample is more applicable for bearing high contact stresses (contact pressure of
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printed sample subjected to lesser contact stresses (contact pressure of 84 MPa). Given the
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32 above, heat-treated samples demonstrate promising applications involving varying sliding
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processes such as cold-extrusion.
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32 Samples
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Figure. 19 shows the 3D surface contours of worn-out surfaces of both the DMLS processed
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38 samples tested against 5 N normal load at all sliding velocities. It is evident from the data that the
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40 wear track width of the as-printed sample is increasing with the higher sliding velocities
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compared to the heat-treated sample (see Table 5), which corroborates well with the trend
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45 observed in Fig. 17 and 18.
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42 Figure. 19 3D surface contours of worn-out surfaces of DMLS processed samples:
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44 as-printed: (a), (b) and (c); heat-treated: (d), (e) and (f)
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3 Table 5: Wear track width of as-printed and heat-treated samples
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7 Sl.no Wear Test Conditions As-Printed (μm) Heat Treated (μm)
8 1 5N, 0.8 m/s 1870 1800
9 2 5N, 1.2 m/s 1850 1700
10 3 5N, 1.6 m/s 1900 1750
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16 Figure. 20 shows the surface roughness measurement results obtained on the wear track shown in
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18 Fig. 19. It could be seen that the as-printed sample had larger roughness values compared to the
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23 (in Fig. 16). The CoF values fluctuations for the as-printed sample can be corroborated with
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25 higher roughness valves, which is presumed due to severe and more material loss via wear debris
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hardness and tensile strength characteristics, the development of contact stresses at the tribo-pair
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32 leads to extensive plastic deformation during the sliding event. Subsequently, it results in deeper
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34 grooves, categorically at higher sliding velocities. Therefore, the generation of higher surface
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roughness on the worn surfaces are observed. However, the heat-treated worn sample had
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39 relatively lower roughness values, which agrees with steady CoF values in the friction curves (in
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41 Fig. 16). In the heat-treated sample, the absence of deeper grooves demonstrates a superior
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43 tribological performance at higher sliding velocities. A similar trend was observed for normal
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46 loads of 10 N and 15 N. Further, it is widely accepted that the protective oxide tribo-film might
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48 have offered a lubricating effect to accord enhanced tribological performance [21].
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4. Conclusions
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34 In the present study, the effect of sliding velocity on the unidirectional sliding wear
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36 characteristics of the DMLS fabricated maraging steel was evaluated in the as-print and heat-
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38 treated conditions. The heat-treated sample had higher hardness (~ 64 %) and higher tensile
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41 strength properties (70-80 %) than the as-printed sample. The wear resistance of the heat-treated
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43 sample found to be three times higher and lower CoF values (~ 24 %) than the as-printed sample
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45 at higher sliding velocities. The tribological enhancement performance was attributed to higher
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hardness and tensile properties of heat-treated samples due to hard intermetallic precipitate phase
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50 and refined microstructure and lubricating oxide tribo-film heat-treated sample at higher contact
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52 stress and sliding velocities.
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1
2
3 References
4
5
6
7 1. Yap, C.Y., Chua, C.K., Dong, Z.L., Liu, Z.H., Zhang, D.Q., Loh, L.E., Sing, S.L.: Review
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46 12. Casalino, G., Campanelli, S.L., Contuzzi, N., Ludovico, A.D.: Experimental investigation and
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50 13. Kang, N., Ma, W., Li, F., Liao, H., Liu, M., Coddet, C.: Microstructure and wear properties of
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3 14. Shakerin, S., Hadadzadeh, A., Amirkhiz, B.S., Shamsdini, S., Li, J., Mohammadi, M.:
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melting. Mater. Sci. Eng. A. 703, 116–123 (2017).
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21 (2016). https://doi.org/10.3390/met6090218
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29 21. Yin, S., Chen, C., Yan, X., Feng, X., Jenkins, R., O’Reilly, P., Liu, M., Li, H., Lupoi, R.:
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32 (2018). https://doi.org/10.1016/j.addma.2018.06.005
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33 22. Yan, X., Huang, C., Chen, C., Bolot, R., Dembinski, L., Huang, R., Ma, W., Liao, H., Liu,
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M.: Additive manufacturing of WC reinforced maraging steel 300 composites by cold
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spraying and selective laser melting. Surf. Coat. Technol. 371, 161–171 (2019).
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38 23. Davis, J.R.: ASM Specialty Handbook{reg_sign}: Carbon and alloy steels. (1995)
39 24. Johnson, K.L.: Contact Mechanics, ISBN 0 521 34796 3. Cambridge University Press, UK
40 (2003)
41 25. Budynas, R.G., Nisbett, J.K.: Eighth Edition in SI Units. 6
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26. Suryawanshi, J., Prashanth, K.G., Ramamurty, U.: Tensile, fracture, and fatigue crack
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Journal name

Influence of Heat Treatment on Microstructure, Mechanical

Journal: Part L: Journal of Materials: Design and Applications

Manuscript Type: Special Issue: Advances in Metal Additive Manufacturing

Date Submitted by the

Materials Design, Materials Testing, Metallic Materials < Materials by

Production < Materials Production

The present work investigates the influence of heat treatment on the

sintering (DMLS) processed maraging steel. The microstructural

determined using a micro-hardness tester and universal testing machine,

27 microstructural examinations were performed using optical microscopy, scanning electron

27 recompenses such as simplified product design approaches, complex geometries, reduction in

27 resistance of DMLS-produced maraging steel. They reported a remarkable improvement in

27 Table. 1. Elemental composition of 18Ni (300) Maraging steel

30 Element Powder (#1) Wt % Splat (#2) Wt %

27 Test Parameters Descriptions

Poisson’s ratio (v2) = 0.3

24 L- longitudinal and T-transverse.

30 3.4.3. Fractography Characterization of Tensile Tested DMLS Samples

27 processed samples (a) as-printed; (b) heat-treated

30 3.5.2. Influence of Sliding Velocity on Worn Surface Topography of DMLS Processed

33 Laser Based Metal Deposition Methodology. Accepted for Publication.

engine Components using Metal Additive Manufacturing. Accepted for Publication

24 by Selective Laser Melting. Metals. 8, 32 (2018). https://doi.org/10.3390/met8010032

24 J. Tribol. 130, (2008). https://doi.org/10.1115/1.2959110

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