Accepted Manuscript

An investigation on D-gun sprayed Al2O3-SiC coatings

Vishal Sharma, Kazi Sabiruddin

PII: S0257-8972(19)30741-8
DOI: https://doi.org/10.1016/j.surfcoat.2019.07.021
Reference: SCT 24797
To appear in: Surface & Coatings Technology
Received date: 1 April 2019
Revised date: 8 July 2019
Accepted date: 9 July 2019

Please cite this article as: V. Sharma and K. Sabiruddin, An investigation on D-gun
sprayed Al2O3-SiC coatings, Surface & Coatings Technology, https://doi.org/10.1016/
j.surfcoat.2019.07.021

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 ACCEPTED MANUSCRIPT

An investigation on D-gun sprayed Al2O3-SiC coatings

Vishal Sharmaa, Kazi Sabiruddina,1

a
Discipline of Mechanical Engineering, Indian Institute of Technology Indore,

Simrol, Indore 453552, India

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Abstract

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Mechanically blended Al2O3-SiC feedstock powder with varying SiC content (0%, 3%, 5%,

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7%) is deposited on AISI 1020 steel substrates by Detonation gun technique. All the coatings

are successfully deposited on the substrate without decomposing SiC in the coating. The
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influence of SiC content on the mechanical properties of the coating is thoroughly studied.
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Through XRD analysis and scanning electron microscopy (SEM) the phases and micro-

structure of the coating are studied respectively. Quantitative phase analysis is performed by

Rietveld refinement technique. Porosity of the coatings is estimated by image analysis

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technique. The wear behaviour of the coating is judged by ball-on-disc type tribometer. The
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micro-hardness and fracture toughness of the coatings are evaluated by using Vickers micro-

hardness tester and scratch tester respectively. Amongst the four different coatings, Al2O3-3
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wt. % SiC coating is found to have the highest fracture toughness and micro-hardness values
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along with minimum porosity. Also, compared to the other three coatings Al2O3-3 wt. % SiC

has shown the highest wear resistant property. Adhesion induced spallation and brittle

fracturing of lamellae are the two main wear mechanisms of the coatings. Phase stabilization

of Al2O3 is found to happen while spraying with 3-5 wt. % of SiC.

Keywords: Alumina; D-gun; Coating; Hardness; Toughness; Wear.

1
Corresponding author. E-mail address: skazi@iiti.ac.in (Kazi Sabiruddin).

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1. Introduction

In aerospace, automotive and petrochemical industries alumina (Al2O3) coated steels are used

for wide range of applications [1]. Alumina coatings added with low quantity of different

materials are frequently used for many applications to improve the resistance against various

types of wear [2, 3]. The alumina coatings are generally hard and chemically stable at high

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temperatures [4, 5]. Thermally sprayed Al2O3 is generally deposited by high-Velocity Oxy

Fuel (HVOF), Detonation Gun (D-gun) spray and Plasma Spray techniques [6]. Oxidation

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and high temperature decomposition of feedstock materials are two major limitations of such

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techniques. It has been reported that D-gun and HVOF are suitable techniques to achieve

coating with minimum oxidation and decomposition of feedstock material, as those offer
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higher velocity and relatively lower spraying temperature [7-9]. Also, D-gun technique is
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favoured over HVOF technique to spray Al2O3 as the residual compressive stress induced by

D-gun technique is higher than the same by HVOF technique [10-12]. In D-gun technique,

combustion of oxygen and fuel gas (acetylene) causes detonation inside the gun barrel,
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resulting in a detonation wave. The spray powder is injected in this detonation wave and the
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powder particles achieve a supersonic velocity (800-1200 m/s) [13-15]. This high velocity

favours to obtain a dense coating. However, the temperature obtained from the combustion of
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the fuel gases is not sufficient enough to melt high melting point materials.
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Thermally sprayed Al2O3 coating contains different phases of Al2O3 such as γ, δ, θ etc.

Among them formation of α and γ is predominant [16]. Depending on the nature of the

feedstock and it’s melting and solidification behaviours these phases form. In most of the

applications the feedstock powder is of only α-Al2O3 and the presence of α-Al2O3 in the final

coating is due to the presence of unmelted/partially melted particles in the stream. On the

other hand the γ-Al2O3 forms due to the rapid crystallization of the melted volume [17]. α-

Al2O3 is superior over the metastable phases of alumina in terms of mechanical properties.

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Hence, to improve the mechanical properties of thermally sprayed Al2O3 in many occasions

dopants are added to the Al2O3 feedstock. Addition of TiO2, Cr2O3, ZrO2 etc. to Al2O3 is tried

by many researchers [18-20]. In very few cases SiC is added to Al2O3 feedstock in thermal

spray applications. One such work is carried out to study the microstructure of Al2O3-SiC

nanocomposite ceramic coating prepared by HVOF technique [21]. However, the mechanical

properties of such coating are not evaluated. In a similar work of same researcher Al 2O3-SiC

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nanocomposite coatings are deposited by both HVOF and APS techniques [22]. The presence

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of SiC is found to increase the α-Al2O3 in the resulting coating prepared by HVOF. Also,

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while depositing on Ni-Al bond coat by both HVOF and APS techniques the Al2O3 phases

obtained in the resulting Al2O3-SiC nanocomposite are of α, γ and θ. However, in this work
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too the mechanical properties of the coatings are not judged. Addition of SiC to Al2O3 for the

preparation of cutting tool is a popular approach, as SiC whiskers provides transformation

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toughening property to the ceramic tool [23]. Being harder in nature SiC enhances the wear

resistance of Al2O3-SiC composites. SiC particles facilitate the grain growth of Al2O3, which
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in turn improves the mechanical property of overall coating [21]. Such property of SiC can be
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beneficial for a coating if it is obtained with its original form. A high chance of
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decomposition of SiC in thermal spray processes makes it an unsuitable material. Therefore,

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it is rare to find thermally sprayed SiC coating in available literature. In the present study,

micron size SiC powder is added to sprayable alumina feedstock in low quantity (3-7 wt. %)
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and deposited on low carbon steel substrates by using detonation gun technique. The effect of

SiC addition on the phases and properties of D-gun sprayed Al2O3 is thoroughly studied in

this work.

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2. Experimental Procedure

2.1 Spray Powders

Alumina powder (25 µm, AMDRY 6060, Oerlikon Metco) is blended mechanically with 3, 5,

7 wt. % SiC powder (22.5 µm, SiC-M, SNAM abrasives Private Limited Chennai, India)

named as A3SiC, A5SiC and A7SiC respectively by using a Retsch (PM 100) blending

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machine to produce homogenous mixtures in normal atmospheric conditions. The average

particle size of Al2O3 powder in the mixture is found to be unchanged.

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2.2 Deposition of coatings

The AISI 1020 steel plates with each of 80 mm × 50 mm × 7 mm are selected as substrate
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materials. The substrates are initially cleaned for 5 minutes by chemical cleaning method.
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The dried substrates are further sand blasted by sand blasting (Sandstorm, model SEC-SB-

9090) technique to achieve an average roughness of 5 µm. Prior to the Al2O3-SiC coating
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deposition a Ni-20 wt. % Cr (METCO 43 C-NS) bond coat is applied on the just cleaned
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rough substrates. The ‘AWAAZ’ D-Gun coating system (SVX Private Limited Noida, India)
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based on combustion of gaseous fuels (oxygen and acetylene) is used for the deposition of

both bond coat and substrate top coat of Al2O3-SiC. The D-Gun is capable of producing 6
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shots/s. On achieving bond coat thickness of approximately 80-100 µm the Al2O3-SiC

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powder mixture is deposited on top of the same and approximately 200-300 µm thickness of

Al2O3-SiC coating is achieved. The process parameters are selected from the literature of

similar works and are shown in Table 1. The loading position of the feedstock powder is kept

in such a way that the particle temperature is not crossed 2400°C. After completion of

deposition the coatings are cooled in normal atmosphere.

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2.3 Characterization of coating

The coated samples are sliced by low speed diamond cutter to obtain multiple numbers of test

coupons with a size of 10 mm × 10 mm × 7.5mm each. The test coupons are ultrasonically

cleaned in acetone bath and subsequently dried. In order to study the microstructure of the

coating cross-section the test coupons are cold mounted and thoroughly polished. A

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unidirectional auto polisher (Struers, LaboPol 25) is used to polish the mounted coating

cross-sections by using SiC polishing papers (wet) with increasing order of mesh size. The

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mirror polished samples are cleaned ultrasonically and then dried samples are used for

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microstructural study. The coating microstructure is studied by inverted microscope (Leica,

DFC 295) and field emission scanning electron microscope (FESEM, Zeiss Supra-55). The
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SEM images are further analysed by Image J software to estimate the porosity of the
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coatings. Atleast 10 images of 10 different locations of the same sample are considered to

find the average porosity of the sample. Phases present in the powder-mixture and in the as-

sprayed coatings are identified by using X-ray diffractometer (Cu-Kα, Rigaku smart lab 3
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KW) with Cu target. The quantity of the phases is estimated by using Rietveld refinement
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method (X’pert HighScore plus, Philips). The measurement of Micro-hardness is done on the

polished cross-sections of the coatings with the help of a Vickers hardness tester (UHL
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Vickers Micro-hardness Tester-002) with 200 gm load and 15s of dwell time. An average of
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at least 10 readings is considered as hardness of each sample. The fracture toughness of the

coating is estimated through scratching the polished top coating (Ra = 0.8 µm) surface by

using a scratch tester (DUCOM , TR- 101) with the help of a Rockwell C diamond indenter

(blue star, tip radius: 200 µm, apex angle: 120°). All the tests are conducted at normal

atmospheric conditions with 50% humidity and 24°C of room temperature. The average

fracture toughness is obtained by considering at least three scratches performed at three

different locations of the same coating surface. A ball-on-disc type tribometer (DUCOM TR-

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20 LE) is used to evaluate wear behaviour of the coatings. The polished (Ra = 0.8 µm) top

surface of the samples with a size of 20 mm × 20 mm × 7 mm each are used to judge the

wear behaviour of the coatings. WC- 6 wt. % Co ball of 6 mm diameter is used as the counter

body for the wear tests. The wear tests are performed under a load of 2.5 Kgf for a track

diameter of 10 mm, speed of 300 rpm and duration of 15 minutes. The width and depth of the

wear track are measured by contact type stylus profilometer (Taylor Hobson, Surtronic 25) to

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calculate the volume loss in order to estimate the specific wear rate. The wear rate is

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estimated by using the following equation [24],

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ωd = (V/dL) × 10-9 ….(1)
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where,

ωd= Specific wear rate in m3/(N.m)

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d = Sliding distance in metres

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L = Normal load in N
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V = Volume of wear track in mm3

Now, V = πAdw ….(2)

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Where, dw = Diameter of wear track in mm

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A = cross- sectional area of wear track in mm2

It is assumed that the wear scar on the tested sample is similar to a circular segment. The

cross- sectional area of wear track ‘A’ can be estimated by using the following equation [24],

A= R2[ Sin-1(hT/2R)0.5 – 0.25 Sin{ 4(Sin-1 (hT/2R)0.5)}] ….(3)

Where,

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hT = avg. depth of wear track in mm

R = Radius of WC ball counterpart in mm.

3. Results and Discussion

3.1 X-ray diffraction (XRD) analyses and Rietveld refinement

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The XRD patterns of the pure Al2O3 and SiC powders are shown in fig. 1 and the XRD

patterns of all the four Al2O3 based coatings are shown in fig. 2. It is noticed in fig. 1 that

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many peaks of ‘SiC’ are coinciding with some significant peaks of Al2O3. On identification

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of phases shown in fig. 2 it is noticed that in all coatings mainly α-Alumina and γ-Alumina

phases are formed. The presence of α-Alumina in the coating is mainly because of the
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presence of the un-melted cores of Al2O3 particles in the coating whereas; the formation of γ-
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Alumina is due to the rapid solidification of the molten droplets on the metal substrate [25].

The broad humps found at 32˚ and 62˚ angles suggest the presence of amorphous phases in
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the as-sprayed coatings. It is found in literature that formation of amorphous phase in any
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thermally sprayed coating takes place due to rapid cooling of coating material [26]. The
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quantity of amorphous phase formed in the coating depends on the process, process

parameters and the coating material. The molten or semi-molten particles with a supersonic
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velocity hit the substrate to form disc shaped splats with larger diameter and producing
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lamellae with large surface area that increases the rate of solidification to form amorphous

phase. Full sintering state of SiC coatings is not been possible to achieve by thermal-spraying

processes till date especially by High-frequency pulsed detonation (HFPD) process [27].

Being unstable at high temperature (more than 2500° C) SiC dissociates in Si and C which

makes it difficult to achieve SiC phase in the resulting coating [28]. Peaks of rhombohedral

SiC in the XRD patterns suggests the retention of SiC phases in the resulting coating with in-

significant dissociation effect. It is observed from the fig. 2 that few Al2O3 peaks are

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overlapped with SiC peaks [29]. Having peaks of both materials at same 2θ angles is the

reason behind this. It suggests the possible presence of ‘SiC’ in the deposited coatings. In

past, a mixture of Al2O3-SiC powders with varying SiC content was successfully deposited

on the steel substrates by using HVOF while keeping the maximum flame temperature at

2400° C [22]. The maximum temperature which can be attained by Detonation Gun process

is approximately 3850°C and it offers a very high velocity of around 800-1200 m/s [30, 31].

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The detonation gun process is able to minimize the decomposition of feedstock powder due

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to lesser time involved in deposition and lower heat generation [32]. The temperature of the

powder particles attained by D-gun process depends on the Xi/L ratio where ‘Xi’ is the axial

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loading position and ‘L’ is the length of gun barrel [33]. In the present work, this ratio is
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maintained at approximately 0.3 which suggests that the flame temperature to be less than

2400° C. Therefore, no decomposition of SiC is occurred. In few past research works, the
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possibility of obtaining thermally sprayed SiC coating without any decomposition is claimed

[34]. From the XRD analysis report shown in fig. 2 it is clear that not only the formation of
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‘SiC’ phase is ensured, but also no evidence of decomposition is obtained. Even if

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decomposition occurred to form compounds of Si and C, it is not been possible to detect

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those by X-ray due to their negligible presence.

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To study the effect of ‘SiC’ addition on the phase of Al2O3 coating Rietveld refinement is
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performed by using the XRD patterns of all the coatings. The major parameters and phases

are shown in Table. 2. In the refinement process the amorphous phase content in the coating

is considered to be negligible for all the samples. Refinement is performed on each sample

for atleast 10 times. Only those results are accepted for which very low (≤ 2) G.O.F

(Goodness of fitment) are obtained. The averages of accepted results are considered to be the

estimated quantity of phases. Further, the change in α-Al2O3 content of the coating against

SiC addition to the feedstock is plotted in fig. 3. The maximum α-Al2O3 formation is noticed

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in A3SiC coating. With further increase in ‘SiC’ content the quantity of α-Al2O3 phase shows

a decreasing trend. The starting α-Al2O3 phase of the powder transforms to γ phase in the

resulting coating due to the rapid solidification of the molten volume. The unmelted/partially

melted volume of Al2O3 particles has retained its α-phase in the coating. The presence of α-

Al2O3 in A0SiC coating is mainly because of retention of unmelted cores of Al2O3 particles

[24]. The increased α-Al2O3 in the Al2O3 coating suggests proper/slow solidification of

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molten volume of Al2O3 [35]. By the addition of 3 wt. % SiC to the Al2O3 feedstock, the

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melting and solidification behaviour of Al2O3 is affected due to the great mismatch of the

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thermal properties between the two materials. As a result slow cooling of solidifying Al2O3

takes place around the deposited ‘SiC’. However, this is only possible if SiC melts and
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deposits as a splat or the Al2O3 melts at lower temperature than its normal melting point. The

selected process parameters are such that the temperature of combustion does not reach to the
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melting point of ‘SiC’. But the results suggests that with same heat content/temperature

A3SiC powder mixture possibly melted at a temperature which is at or below 2400°C. For
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given process parameters this specific temperature of ‘SiC’ can be reached when the
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feedstock quantity of SiC is close to 3 wt. %. When the feedstock quantity of SiC is more
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than 5 wt.% , with same process parameters/energy input the ‘SiC’ is not been able to get the
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desired temperature for melting or stabilization of Al2O3 phase through slow cooling.
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3.2 Microstructure Study

The SEM micrographs of the pure Al2O3 powder and Al2O3-SiC powder mixtures are shown

in fig. 4. The irregular and angular shaped pure Al2O3 powder (AMDRY 6060) suggests that

the powder was manufactured by crushing. Also, no significant change in the size of Al2O3

powder is noticed on mixing with hard ‘SiC’. The very low quantity of ‘SiC’ possibly could

not cause much harm to the final size of Al2O3 particle. The micrograph of SiC powder shows

the irregular and crushed nature of SiC particles. The micrographs of the coatings are shown

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in fig. 5(a-d). All the coatings are well adhered to Ni-20Cr bond coat. Voids, cracks and

defects are observed in all the coatings. Among all, A3SiC coating shows the minimum

defects present in it. With further increase in the quantity of SiC, the formation of voids,

cracks and defects increases. Pure Al2O3 coating contains more defects mainly due to the

presence of partially melted Al2O3 particles. Partial melting is a commonly observed

phenomenon in thermally sprayed Al2O3 [24]. In D-Gun coating, as the residence time is less

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mostly the Al2O3 particles experience partial melting and due to the presence of unmelted

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portion the defect of the coating increases. This is one of the major reasons for the retention

of starting phase of Al2O3 (in the present study α-Al2O3) in the final coating. On polishing,

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those loosely adhered unmelted cores of Al2O3 particles are removed from the surface and
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deep pockets are exposed. These deep pockets or defect marks are termed as ‘crater marks’ in

the manuscript. Severe defect is observed in A7SiC coating as shown in fig. 5. Through EDS
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mapping of A7SiC, presence of SiC is traced in a limited zone as shown in fig. 5(d). The

small area coverage of Si rich zone suggests the entrapment of unmelted ‘SiC’ particle in
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such coating. The embedded ‘SiC’ particle probably has hindered the proper growth of Al2O3
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crystals surrounding it. In addition, the blasting/bombardment effect of unmelted SiC

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particles on the A7SiC coating surface is also an important factor for increasing defects. The
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presence of SiC in the A3SiC coating is confirmed by EDS analysis as shown in fig. 6. The

bright part in the fig. 6 represents the ‘Si’ rich zone. Also the wavy nature of the zone
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suggests the formation of SiC splat. The splat formation suggests the melting of SiC in

A3SiC coating.

In Thermal Spraying, coating porosity is an important aspect to study as the mechanical

properties depend on it [36]. The detonation process is an intermittent process due to which

few pores get developed in the coatings [13]. An average of at least 10 readings is considered

to estimate the porosity of each sample and presented in fig. 7. The low porosity (<2%) of the

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coatings suggests the impact velocity of the droplets to be very high by the D-gun process [7,

37]. It is evident from fig. 7 that the porosity first decreases and then increases with an

increase in the SiC content. The minimum porosity of about 0.4% is achieved when 3 wt. %

SiC is added to the Al2O3 feedstock. This is due to the increased formation of α-Al2O3 phase

with the improved the wettability property of the deposited droplets. With high spreading of

splats dense coating is achieved. On the other hand, because of bombardment effect and

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inclusion of few ‘SiC’ particles the porosity of A7SiC coating is the maximum.

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3.3 Micro-hardness test

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The Vickers micro-hardness tests are carried out on the polished cross-section of the coatings
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with a load of 200 gm. The average hardness value of each sample is calculated by

considering at least 10 indentations with the same load. The micro-hardness values of all
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coatings are graphically shown in fig. 8. Among all, the A3SiC coating is found to be the

hardest. The coating hardness decreases significantly with further increase in SiC content.
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One of the reasons of such behaviour is the density of the coating which is the maximum for
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A3SiC coating. With more than 3 wt. % SiC content as the density of the coating decreases,
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the hardness of the same decreases too. However, as we have observed (fig. 7) very low
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change in porosity (˂ 1%) of the coatings, density cannot be the only reason for the

significant change in hardness. Therefore, other reasons for such behaviour are to be found
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out. It is well known that amongst different phases of Al2O3 the stable α-phase possess the

highest mechanical properties [24, 38]. Hence, more the presence of α-Al2O3 in the coating

more will be the hardness. The Vickers indentation marks of all the samples are shown in fig.

9. The cracks formed at the corners and edges of the rhomboidal indent mark on A3SiC are

the minimum among all. The presence of SiC splats helps to restrict the

formation/propagation of cracks [39]. On the other hand, the indent marks created on A0SiC

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coating and A7SiC coating show higher crack formation due to their high brittleness

properties owing to high γ-Al2O3 content. The highest quantity of α-Al2O3 together with few

molten/semi-molten ‘SiC’ makes the A3SiC coating to be hardest and toughest among all.

3.4 Fracture Toughness by Scratch tests

Fracture toughness of the coating is estimated by scratching the polished coating surface with

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conical diamond indenter. The applied load and scratching speed used during the tests are of

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15 N and 0.1 mm/s respectively. Fracture toughness (Kc) of the coating is evaluated by using

following equation [40].

Kc = Feq/ (2pA)0.5…(1)
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Feq = (FT2 + 0.6 FV2)0.5
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(2pA)0.5= (4d3 [Tan Ø / Cos Ø] )0.5 For Conical Probe

Where, Kc = Fracture toughness

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Feq = Contributions of both the vertical and the horizontal forces

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(2 pA) = Scratch probe shape function {p= Perimeter of indenter; A= Area of indenter}

FV = Vertical force
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FT = Horizontal force
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Ø = Half-apex angle of conical indenter

d = Penetration depth

The average fracture toughness values of the coatings are graphically shown in fig. 10 and the

SEM images of scratch marks are shown in fig. 11. The scatter of fracture toughness values

observed in this work represents the non-homogenous nature of the coating micro-structure

[10]. The A3SiC coating shows the highest fracture toughness property among all four

coatings. With further increase in SiC content in the feedstock the toughness of the coating

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reduces significantly. ‘SiC’ imparts toughness property to the coating through transformation

toughening. It also possesses crack deflection property. To achieve these properties in the

coating the primary condition is to include the ‘SiC’ in the coating as a splat with proper

adhesion. Inclusion of well adhered ‘SiC’ in the coating is reduced as the quantity of SiC

increases in the feedstock. This is due to the limited energy input by D-gun process. Also, the

high velocity unmelted ‘SiC’ particles have caused damage to the coating to form a non-

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homogenous coating micro-structure. The high scatters obtained in the results of A5SiC and

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A7SiC suggests these coatings to be non-homogenous in nature.

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3.5 Ball on disc type wear test
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Ball on disc type wear test is carried out on the polished (Ra=0.8 µm) top surfaces of the

coatings with an average thickness of 250 µm each. The specific wear rate of the coatings is
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shown in fig. 12 and the depth profiles of the wear tracks are shown in fig. 13. The specific

wear rate is reduced significantly from A0SiC to A3SiC coating. Also, further increase in SiC
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content results in rapid wear of coating materials. From the depth profiles of wear track
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shown in fig. 13 it is observed that the depth of wear track is the minimum for A3SiC
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coating. Also, the maximum value of the same is obtained for A7SiC coating. The
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irregularities on the track wall are more in both A0SiC and A7SiC coatings. A sudden

increase in depth is observed in the wear track of A7SiC coating due to the dislodgement of
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embedded SiC particle from the track depth. On the other hand, smoother track walls are

found in case of A3SiC and A5SiC coatings which are due to the ductile nature of the

coatings showing some plastic deformation prior to the material flow.

The microscopic images of the worn surfaces of all the coatings are shown in fig. 14. The

distinguished wear tracks of the coatings suggest the major mode of failure to be spallation.

Under cyclic loading condition fatigue stress developed on the deposited splats which

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resulted in the formation of fatigue cracks in the transverse direction of the wear tracks.

Being brittle in nature the coating material helps the crack to propagate quickly across the

wear tracks and between two splats of similar lamellae. The cyclic loading of the coating

surface leads to crack propagation along the splat boundary due to which material spallation

has taken place. Spallation or delamination is the major mode of adhesive failure observed in

both A0SiC and A5SiC coatings. On the other hand, for A7SiC coatings, in the first few

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cycles the defects are exposed and spallation has occurred. With further loading in next few

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cycles the embedded SiC particles are dislodged and entrapped in between the work surface

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and WC ball. This leads to start three body wear mechanism due to the abrasive action of

those entrapped SiC particles. The next major portion of material removed from A7SiC
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coating is due to abrasion. The severe scratch grooves and furrows formed in the longitudinal

direction of wear track suggest the major mode of wear for A7SiC coating is to be abrasive.
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A very less amount of spallation is noticed on the wear track of A3SiC coating. The burrs

formed due to ploughing action of the WC ball are visible at the edges of wear track (fig.
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14(b)). This suggests the improved ductility and toughness of A3SiC coating material. In the
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later stage of cyclic loading action few spalled off hard particles have caused abrasion to the
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surface. The fine scratches and furrows are in good agreement with this. Due to the ductile
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nature of the coating material, separation of material is little in case of A3SiC coating.
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The magnified view of wear debris collected from all samples is shown in fig. 15(a-d).

The powder nature of debris of A0SiC coating suggests that mostly loose unmelted particles

are detached from the wear track. Broken laminar fragments along with few powder type

debris are observed in case of A3SiC coating. This suggests the removal of solidified splats

along with unmelted powder of Al2O3. However, having comparatively low quantity of

unmelted Al2O3 particles suggests good melting of Al2O3 in A3SiC coating. In case of

A5SiC, the quantity of unmelted particles is increased. Therefore, in the debris both broken

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fragments and fine particles are observed equally. Debris of mostly fine particles and few

lamellar fragments are observed in case of A7SiC coating. In addition, few ‘SiC’ particles are

also observed in the debris. The EDS analysis confirms the presence of Si and C in the debris

of A7SiC.

In D-Gun coated Al2O3, due to low heat generation and less dwell time the Al2O3 particle

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experiences partial melting. However, with a very high velocity those unmelted particles

spread well and dense coating is achieved. With addition of low quantity ‘SiC’ to Al 2O3

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feedstock significant change in porosity, hardness and wear behaviour is observed in the

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Al2O3 coatings. The selected process parameters are not sufficient to melt ‘SiC’ as its melting

point is much more than the same of Al2O3. Also, the thermal conductivity and toughness of
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SiC are higher. For the given process parameters/heat content the 3% SiC is the optimum

quantity to add with Al2O3 feedstock for the deposition of ‘SiC’ splats. This improves the α-
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Al2O3 phase formation and toughness of the overall coating. With enhanced α-Al2O3 quantity

the hardness of the coating is enhanced. Also, the well adhered ‘SiC’ of A3SiC coating
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imparts toughness to the coating material. However, with given heat input further increase in
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SiC addition to Al2O3 feedstock is not been able to deposit ‘SiC’ in splat form. Therefore,

enhancement of the α-Al2O3 phase content and so the properties of coating are not noticed.
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The limited energy produced in per shot has restricted the amount of melting volume of SiC.
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The few ‘SiC’ particles embedded in A5SiC and A7SiC coatings makes weak bond with the

surrounding Al2O3. Also, with high velocity some of the unmelted SiC particles have

bombarded the just deposited Al2O3 coating and created defects. The improved α-Al2O3 phase

content by addition of 3 wt. % SiC suggests the stabilization of Al2O3 phase in A3SiC

coating. The enhanced mechanical properties of such coating once again supports the fact of

improvement in α-Al2O3 phase content. As the addition of SiC is very less, the significant

improvement in mechanical properties is not due to the presence of ‘SiC’ in such coating.

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4. Conclusions

1. Al2O3-SiC can be successfully deposited on Ni-20Cr bond coated AISI 1020 steel samples

by D-Gun technique without decomposing SiC. Dense coatings of Al2O3-SiC are obtained

with less than 2% of porosity.

2. A very low quantity of ‘SiC’ is found to affect the melting and solidification behaviour of

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D-gun sprayed Al2O3. Deposition of ‘SiC’ helps to improve the α-Al2O3 phase content of

A3SiC and A5SiC coating.

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3. With highest hardness and toughness properties A3SiC is found to be the highest wear

resistant material among the selected coatings.

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4. For selected process parameters, more than 3% of ‘SiC’ addition to the feedstock tends to
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decrease the mechanical properties of Al2O3 coating. The high velocity unmelted ‘SiC’

particles damage the just solidified Al2O3 by bombardment.

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5. Phase stabilisation of Al2O3 is possible in D-gun sprayed coating with 3-5 wt. % of SiC
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addition to the Al2O3 feedstock.

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Acknowledgements
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The authors would sincerely like to thank the Field-Emission Scanning Electron Microscope
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(FE-SEM) and Powder X-ray Diffraction (P-XRD), Facility equipped at Sophisticated

Instrument Centre (SIC), IIT Indore. The authors would sincerely like to thank the staff and

members of the Metallography and Tribology Laboratory, Department of Mechanical

Engineering, IIT Indore, for their involvement in the work. Financial support from MHRD is

gratefully acknowledged.

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Table 1: Detonation gun parameters used in this investigation.

Parameters Details

Oxygen flow rate (SLPH) 4800

Acetylene flow rate (SLPH) 1920

Nitrogen flow rate (SLPH) 800

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Spray Distance (mm) 200

Oxygen pressure (Mpa) 0.2

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Acetylene pressure (Mpa) 0.14

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Nitrogen pressure (Mpa) 0.4

Air pressure (Mpa) 0.4

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Table 2: Parameters used during Rietveld refinement

ICSD ICDD Name Chemical Space a[A°] b[A°] c[A°] α[°] Β[°] γ[°] Z
formula group
26790 01- Aluminum Al2O3 R-3c 5.1280 5.1280 5.1280 55.2700 55.2700 55.2700 2
074- Oxide (α)
1081
85137 01- Aluminum Al2O3 R-3c 4.7607 4.7607 12.9970 90.00 90.00 120.00 6
088- Oxide (α)
0826
39014 01- Aluminum (Al2O3)1.333 Fd- 7.9060 7.9060 7.9060 90.00 90.00 90.00 8

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077- Oxide (γ) 3m
0396
30267 01- Aluminum (Al2O3)1.333 Fm- 3.95000 3.95000 3.95000 90.00 90.00 90.00 1.00

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075- Oxide (γ) 3m
0921
43727 01- Silicon SiC R3m 3.0790 3.0790 438.2000 90.00 90.00 120.00 174

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089- Carbide
3067
42868 01- Silicon SiC R3m 3.0730 3.0730 218.6570 90.00 90.00 120.00 87
089- Carbide
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List of Figures

Figure 1 XRD Patterns of the pure Al2O3 and SiC powders

Figure 2 XRD patterns of D-gun sprayed Al2O3-SiC coatings

Figure 3 Change in percentage of α-alumina with change of SiC content in feedstock

powder

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Figure 4 Morphology of (a) A0SiC (b) A3SiC (c) A5SiC (d) A7SiC powders.

Figure 5 SEM images of different coatings at lower magnification (a) A0SiC (b)

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A3SiC (c) A5SiC (d) A7SiC

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Figure 6 EDS analysis of A3SiC coating
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Figure 7 Percentage porosity graph of coatings

Figure 8 Microhardness graph of coatings with different SiC content

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Figure 9 Micrographs of Vickers indent marks produced by applying 200gm of load

on the cross-section of (a) A0SiC (b) A3SiC (c) A5SiC (d) A7SiC coatings
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Figure 10 Fracture Toughness graph coatings with different SiC content

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Figure 11 Microscopic images of scratch marks produced on (a) A0SiC (b) A3SiC (c)
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A5SiC (d) A7SiC coatings

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Figure 12 Specific wear rate of the coatings.

Figure 13 Depth profiles of wear tracks of (a) A0SiC (b) A3SiC (c) A5SiC (d) A7SiC
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coatings.

Figure 14 Wear track images of (a) A0SiC (b) A3SiC (c) A5SiC (d) A7SiC coatings

captured by inverted microscope.

Figure 15 SEM micrographs showing wear debris of (a) A0SiC (b) A3SiC (c) A5SiC

(d) A7SiC coatings.

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Highlights

 Al2O3-SiC powder mixture with low SiC content can be successfully deposited on Ni-

20Cr bond coated AISI 1020 steel samples by D-Gun technique without decomposing

SiC.

 With improved hardness and toughness properties Al2O3-3wt% SiC coating is found

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to be the highest wear resistant material among the selected coatings.

 Up to 5wt.% of SiC addition to the Al2O3 feedstock improves the mechanical

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properties of D-Gun coated Al2O3.

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