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Influence of Grit Blasting on Residual Stress Depth

Profile and Dislocation Density in Different Metallic


Substrates
TINA GHARA, S. PAUL, and P.P. BANDYOPADHYAY

This work deals with the effect of grit blasting on the surface and in-depth properties of a
number of commercially available metals/alloys, i.e., low carbon steel, C45 steel, SS316,
Ti-6Al-4V, Inconel 718, and Hastelloy X. The residual stress depth profile and dislocation
density of the specimens were determined using X-ray diffraction. A substantial increase in
dislocation density was observed after grit blasting. A transmission electron microscope was
utilized to observe the dislocation structure in a grit-blasted specimen. Strain hardening was also
observed at the blasted surface owing to dislocation interaction and entanglement. The hardness
profile followed a trend similar to that of dislocation density along the depth of grit-blasted low
carbon steel. Moreover, compressive residual stress is induced in the blasted surface having a
maximum value at a certain depth. The maximum induced compressive residual stress was
found to have a good correlation with the Johnson–Cook flow stress. Moreover, the depth of
the affected layer and the increase in hardness were found to depend on the yield strength and
the strain hardening exponent of the materials, respectively. A plastic deformation-induced
phase transformation from austenite to martensite was also identified in the case of SS316.

https://doi.org/10.1007/s11661-020-06055-x
 The Minerals, Metals & Materials Society and ASM International 2020

I. INTRODUCTION materials in thermal spraying applications.[6,7] Carbon


steels are extensively used as the structural materials,
SURFACE preparation is an important and integral whereas SS316 and Ti-6Al-4V are utilized as medical
part of the thermal spraying process and is performed implants.[8] On the other hand, Ni-based superalloys are
prior to deposition of thermally sprayed coatings.[1–3] mostly suitable for high temperature applications, i.e.,
This is accomplished using various means to make the turbine blades, heat exchanger tubes, jet engines, and so
surface suitable for deposition of coatings. Grit blasting on.[9]
is a surface preparation technique in which sharp Grit blasting is the most common process that is
abrasive grits are made to impinge on to the substrate employed to remove scales and deposits from the
surface at a high velocity. Upon impact, the hard grit substrate surface.[10,11] Grit blasting is also useful to
erodes a small volume of material leaving a small crater improve the fatigue life of the substrates.[12,13] Cattoni
on the surface. Repeated occurrence of such impacts et al.[14] reported that grit blasting restricted fatigue
results in roughening of the substrate surface.[4] The crack initiation and growth owing to the generation of
rough surface thus produced is often useful for better compressive residual stress in Ti-6Al-7Nb and AISI
mechanical anchorage of the coating and the sub- 316LVM substrate surfaces.
strate.[5] Alumina, silicon carbide, SiO2, ZrO2, B4C, Different material removal mechanisms in surface
diamond, etc., are commonly used grit materials. erosion by abrasive particles were observed by various
Considering the material chemistry, excellent struc- researchers.[15,16] Chander et al.[17] observed that micro-
tural properties, and wettability, low carbon steel, cutting and shearing of the low carbon steel surface after
stainless steel, Ti-6Al-4V, high carbon steel, Nimonic, grit blasting. They also investigated the influence of grit
Hastelloy, Inconel, etc., are prevalently used as substrate blasting parameters on surface properties like rough-
ness, residual stress, and hardness. Staia et al.[18] exam-
ined the adhesive property of the WC-Co coating on the
basis of surface roughness of the grit-blasted substrate.
TINA GHARA, S. PAUL, and P.P. BANDYOPADHYAY are They observed that a rougher surface is capable to
with the Department of Mechanical Engineering, Indian Institute of provide better anchorage with the coating material.
Technology Kharagpur, Kharagpur, West Bengal 721302, India.
Contact e-mail: ppb@mech.iitkgp.ac.in
A grit-blasted surface usually harbors a compressive
Manuscript submitted March 23, 2020; accepted October 5, 2020. residual stress. The residual stress becomes more com-
Article published online October 30, 2020 pressive at a certain depth, and then, it gradually

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—65


decreases to near zero value with the depth. A plot of diffraction of each material using Williamson–Hall
residual stress vs depth is known as residual stress depth method. Dislocation density profile was also obtained
profile. The depth profile of the residual stress (com- along the depth of annealed grit-blasted low carbon
pressive in the case of grit blasting) affects the crack steel. To the knowledge of author, such an in-depth
growth from the surface to the interior of a grit-blasted investigation considering so many aspects of grit blast-
component. This aspect has been investigated by several ing has not been reported so far. The data available in
researchers. Mellali et al.[19] utilized bending method the literature are scattered and few. Therefore, it was felt
and incremental hole drilling method to estimate the appropriate to conduct a comprehensive investigation
residual stress in grit-blasted aluminum alloy AU4G, on the properties of a few important alloys in
hard carbon steel 100C6, and cast iron FT25. Pressure, grit-blasted condition using the same set of equipment
grit size, and substrate material properties influenced the and instruments.
depth of the affected zone after grit blasting. In case of
FT25 substrate, the maximum compressive residual
stress was found to be around 600 MPa at a depth of II. MATERIALS AND METHODS
approximately 30 lm from the surface. Kovářı́k et al.[20]
measured residual stress in alumina-blasted low carbon A. Materials
steel using neutron diffraction method. A maximum The alloys selected for grit blasting along with their
compressive residual stress of 100 MPa was induced at nominal chemical compositions are listed in Table I.
around 50 lm under the blasted surface. The hardness Test samples of size 15 9 15 9 5 mm were cut off from
of the blasted surface also increased after grit blasting. larger plates. Two coupons from each set of materials
The substrate material is severely deformed under grit were annealed in a vacuum tubular furnace (Nisabjee
blasting treatment. This deformation, in turn, results in Engg. Co., Kolkata, India), following specific annealing
an increase in the dislocation density in the deformed cycles for individual materials. The annealing cycles
region. Dislocation density is expected to increase in a applied on different materials are tabulated in Table II.
material that is subjected to mechanical working such as In all cases, furnace cooling of the samples was done
machining, rolling, shot peening, grit blasting, and so after the annealing operation.
on. Wu and Jiang[21] calculated the dislocation density in
shot peened Inconel 625. An increase in the dislocation
density from around 1 9 1013 m2 to around 791014 B. Grit Blasting
m2 was observed using Williamson–Hall method. Fu Both as-received and annealed samples for each
et al.[22] also estimated dislocation density in SS304 after material were grit blasted in a suction type grit-blasting
triple step shot peening using the said method. The machine (SANDSTORM, Bangalore, India) using
maximum dislocation density of around 1016 m2 was Al2O3 grits of mesh size #24 (704 lm). The following
found after shot peening process. The dislocation parameters were used for blasting purpose: pressure 7
density was increased by two orders in this case. bar, SOD 120 mm, nozzle angle 90 deg, and blasting
Reports on residual stress in grit-blasted components time 60 seconds. The grit-blasted specimens were then
are few. Even fewer reports are available on residual cleaned ultrasonically after dipping them into 2-propa-
stress depth profiling. In fact, no work was found in the nol to clean the grit residue[28] present on the blasted
literature on residual stress depth profiling of grit- surface.
blasted Ni-based materials such as Inconel 718 and
Hastelloy X. Moreover, to the knowledge of the
authors, no report on dislocation density in grit-blasted C. Characterization of Specimens
metallic substrates is available in the literature. In After grit blasting, the morphology of the blasted
addition, no dislocation density depth profile of the surfaces was observed under SEM (EVO 15, Zeiss, Jena,
grit-blasted material was found in the literature. Germany). A contact-type surface roughness tester
In this work, residual stress depth profiling of a set of (TALYSURF 50, 3D profilometer, TAYLOR HOB-
widely used and important substrate materials after grit SON, UK) was used to measure the roughness of the
blasting were undertaken. The selected substrate mate- blasted surfaces. The traverse and cut-off lengths for
rials are low carbon steel, C45 steel, SS316, Ti-6Al-4V, surface roughness measurement were set at 4 and 0.8
Inconel 718, and Hastelloy X. The stress depth profile mm, respectively. The roughness measurement was
was acquired by measuring the residual stress using performed at five places on the blasted surface and an
X-ray diffraction after successive removal of the sub- average of those five readings is presented.
strate layers by electropolishing. The maximum com- X-ray diffraction patterns of all the materials, prior to
pressive stresses in different materials were correlated and after grit blasting, were acquired by scanning a 2h
with Johnson–Cook flow stress. In addition, hardness range of 20 to 160 deg using Cu–Ka radiation. There-
depth profile in each case was obtained at the polished after, background correction and Ka2 stripping were
cross-sections of the grit-blasted samples. The depth of applied in all the X-ray diffraction profile for the line
affected layers and the percentage increase in hardness profile analysis as discussed by Delhez et al.[29] Then, the
were correlated to the yield strength and strain harden- average crystallite size and microstrain were obtained
ing exponent of the materials, respectively. Further- using Williamson–Hall[30,31] equation, considering uni-
more, the dislocation density of as-received, annealed, form deformation model (UDM). It was assumed that
and grit-blasted specimens were estimated from X-ray

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Table I. Nominal Compositions of Different Materials Under Consideration

Elements Fe C P Mn S
[17]
Low Carbon Steel (Wt Pct) balance 0.2 0.04 0.3 0.05

Elements Fe C Mn Si Cr P S Mo Ni Cu Al
[23]
C45 Steel (Wt Pct) balance 0.45 0.65 0.25 0.4 0.008 0.025 0.1 0.4 0.17 0.01

Elements Fe C Cr Ni Se Si Mn Mo
[24]
SS316 (Wt Pct) balance 0.02 16.3 10.2 5.4 0.455 1.5 2.08

Elements Ti Al V Fe C O H N
[25]
Ti-6Al-4V (Wt Pct) balance 6.08 4.02 0.22 0.02 0.18 0.0053 0.01

Elements Ni Cr Mo Nb Fe Co Cu Ti Al C
[26]
Inconel 718 (Wt Pct) balance 19.06 3.04 5.08 18.15 0.11 0.02 0.93 0.52 0.021

Elements Ni Cr Fe Mo Co Mn Si W C
Hastelloy X[27] (Wt Pct) balance 22 18 9 1.5 1 1 0.6 0.1

Table II. Detail of Annealing Cycles

Material Temperature (C) Heating Rate (C/min) Dwell Time (h)


Low Carbon Steel 500 6 1
C45 Steel 400 6 1
SS316 400 6 1
Ti-6Al-4V 700 6 1
Inconel 718 550 6 1.5
Hastelloy X 600 6 2

the strain is uniform along all the crystallographic In case of BCC crystal, most favorable slip plane is of
directions. The Williamson–Hall equation is given by, {1 1 0} type and the slip direction is of h1 1 1i type. The
kk Burgers vector is expressed as follows: b~ ¼ a2 h111i,
b cos h ¼ þ 4e sin h ½1 where a is the lattice
  constant. Therefore, the magnitude
D pffiffi
~ a pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
of the vector is b ¼ 2 1 þ 1 þ 12 ¼ 23a. Similarly, in
2 2
where 2h is the position of the peaks, b is FWHM of
different peaks, k is shape factor (k = 0.9), k is the the case of FCC crystal, most favorable slip plane and
wavelength of X-ray (k = 1.54 Å), D is crystallite size, direction are of {1 1 1} and h1 1 0i types, respectively.
and e is microstrain. The values of D and e are calcu- Therefore,
 the Burgers vector is b~ ¼ a2 h110i and
lated from the intercept and slope, respectively, from ~ a pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
b ¼ 2 12 þ 12 þ 02 ¼ paffiffi. On the other hand, for
b cos h vs 4 sin h plot. The dislocation density of the 2
blasted and non-blasted specimens was then estimated HCP crystal, most favorable slip plane  is the basal
using the following formula,[21,22] plane and the direction is of 1120 type. Hence, the
pffiffiffi 1=2 Burgers vector is b~ ¼ a3 h11
20i and
2 3 e2   qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi pffiffi
  ~ a 2
q¼ ~ ½2 b ¼ 3 12 þ 12 þ ð2Þ þ02 ¼ p2ffiffi3a, where a is the basal
bD lattice parameter. Table III lists the calculated values of
    the Burgers vector of the considered materials.
   
where b~ is the Burgers vector. The Burgers vector (b~) Grazing incidence X-ray diffraction pattern of SS316
signifies the distortion in a crystal lattice that is is obtained by Cu Ka radiation in 40 deg £ 2h £ 55 deg
generated owing to dislocation. It is denoted as the with an incidence angle of 1 deg and 0.03 deg step size
shortest lattice translation vector along the slip direction to examine the formation of deformation-induced
in a most favorable slip plane (closely packed plane). martensite.
The Burgers vectors were calculated considering a The blasted and non-treated specimens were cross
(BCC lattice) peaks for low carbon steel and C45 steel, a sectioned, polished, and metallographically etched to
(HCP lattice) peaks for Ti-6Al-4V and c (FCC lattice) obtain cross-sectional views. The prepared cross-sec-
for SS316, Inconel 718 and Hastelloy X. tions were utilized for microhardness measurement as

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—67


well. A Leco LM 700 microhardness tester was utilized Thereafter, the residual stress corrected for stress
for hardness testing using a load of 50 gf with a dwell relaxation is plotted to construct the residual stress
time of 15 seconds. The hardness measurement was depth profiles.
performed along the thickness of the specimens to Dislocation density depth profile of grit-blasted low
obtain hardness depth profile. Ten measurements were carbon steel was also obtained by measuring the density
taken at a particular depth and their average along with each time after successive material removal by
standard deviation is presented. electropolishing.
The residual stresses of both blasted and non-blasted A transmission electron microscope (TEM)
surfaces were measured using X-ray diffraction tech- (JEM-2100F, JEOL, Tokyo, Japan) was employed to
nique in a high-resolution XRD machine (PANalytical, observe the dislocation structure of the annealed and
Empyrean, DY1705, Netherlands).[32,33] Cu tube grit-blasted (after annealing) low carbon steel speci-
(Empyrean Cu LFF HR (9430 033 7310x) DK411025) mens at a depth of 50 lm from the treated surface.
generating Ka radiation was used for Ti-6Al-4V, The samples were cut parallel to the surface at a depth
whereas for other materials, Cr tube (Empyrean Cr of 1 mm using a low-speed CBN cutter in a
LFF (9430 033 7800x) DK411025) was employed. STRUERS machine (Copenhagen/Denmark). The
However, the other settings in the optics of the XRD sliced samples were thereafter electropolished to
machine were kept same for both targets. A point source remove a layer of thickness 50 lm from the top
with a parallel beam X-ray lens having mask of 2 mm surface. Then, the opposite sides of the samples were
and divergence slit of 4 mm was employed in the polished using SiC polishing papers to a thickness of
incident beam side of the diffractometer. An open around 70 lm. After that, a disk of 3 mm diameter
detector with parallel plate collimator was employed in was cut out from each of the polished samples. Next,
the diffracted beam side. The instrument was operated a dimple of 1 mm diameter was made in the centers of
at 30 kV and 55 mA for Cr target material and at 45 kV the samples using a GATAN 656 (Pleasanton, CA)
and 40 mA for Cu target material. The stress measure- dimple grinder. The thickness of the sample at the
ment was undertaken using sin2w method with a step dimpling area was brought down to around 30 lm.
size of 0.1 and taking eleven stage tilt angles (0 deg, Thereafter, the samples were further thinned and
± 18.43 deg, ± 26.57 deg, ± 33.21 deg, ± 39.23 deg, polished by ion milling using a GATAN (Model No.
and ± 45 deg) from 45 to 45 deg. The diffraction 691) ion polishing machine at an incident angle of 3 to
angle ranges utilized for stress measurement of each 4 deg, till a hole appears in the sample. TEM
material under consideration is given in Table IV. observations were made near the edge of the perfo-
Evaluation of residual stress was performed by stress rated area where the material thickness was around
analysis software (Panalytical B.V., Almelo, Nether- 100 nm or less.
lands) through fitting the data by straight line. Stress
measurement was undertaken at two different positions
on every sample surface and the average of these two III. RESULTS
measurements with error bar is presented.
Residual stress depth profiling was accomplished by A. Morphology and Surface Roughness
removing successive layers of the grit-blasted samples SEM images of blasted surfaces reveal an irregular
from the top by electropolishing, followed by stress rough surface resulted from grit blasting with alumina
measurement on the exposed layer. For this purpose, a grits. The morphology of the grit-blasted surfaces,
BUEHLER electropolisher cell module (ElectroMet 4) observed under scanning electron microscope, is shown
was used. Up to a depth of around 100 lm, an approx- in Figure 1. The images also show microcutting and
imately 20 lm thick material layer was removed every indentation marks on the blasted surface. The traces of
time. Thereafter, the layer thickness was kept around 40 indentation and microcutting are shown in the figure by
lm. Table V shows the electrolyte and parameter com- yellow and red arrows, respectively. Average surface
binations for different alloys considered in this work. roughness of the grit-blasted surfaces is tabulated in
The material removal is associated with relaxation Table VI.
and redistribution of the residual stress. Therefore, Scanning electron images of alumina grit of 24 mesh
correction is necessary on the measured stress values to size utilized for grit blasting are shown in Figure 2. It
determine a more accurate stress profile. Considering can be observed from the figure that the abrasive grits
small depths of material removal, the corrected residual also underwent erosion after repeated blasting.
stress r(z) at a depth z can be expressed the following
equation as proposed by Moore and Evans[34]:
  B. Cross-Sectional Microstructure
Dz
rðzÞ ¼ rm ðzÞ þ ð4Þ  rm ðHÞ  ½3 Grit blasting deforms the material plastically by
H
repeated impact on the substrate surface. Figures 3((a)
where rm ðzÞ, rm ðHÞ, H and Dz are the measured residual to (b)) exhibit the cross-sectional view of low carbon
stress at depth z, measured residual stress before surface steel specimen prior to and after grit blasting. The
removal, original thickness of the sample, and thickness figure depicts deformation of ferrite and pearlite phases
of material removed, respectively. near the blasted surface.

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Table III. Crystal Lattice and the Associated Values of the Burgers Vector for Different Metallic Materials
 
 
Materials Crystal Lattice Burgers Vector (~
b) (nm)
Low Carbon Steel BCC 0.248
C45 Steel BCC 0.248
SS316 FCC 0.258
Ti-6Al-4V HCP 0.241
Inconel 718 FCC 0.250
Hastelloy X FCC 0.250

Table IV. Ranges of Diffraction Angles Used for Stress Measurement

Materials X-Ray Source 2h Range Crystallographic Plane (h k l)


Low Carbon Steel Cr 151.93 deg < 2h < 160.93 deg (2 1 1)
C45 Steel Cr 152.22 deg < 2h < 160.22 deg (2 1 1)
SS316 Cr 124.61 deg < 2h < 132.61 deg (2 2 0)
Ti-6Al-4V Cu 135.01 deg < 2h < 147.01 deg (2 1 3)
Inconel 718 Cr 125.25 deg < 2h < 130.25 deg (2 2 0)
Hastelloy X Cr 125.2 deg < 2h < 130.2 deg (2 2 0)

Table V. Electrolyte and the Parameter Combinations Utilized for Electropolishing

Amount of
Material
Materials Electrolyte Voltage (V) Time Removed (lm)
[35]
Low carbon steel 50 pct H3PO4+ 20 pct H2SO4+ 30 pct H2O 15 1 min 20
C45 steel 50 pct H3PO4+ 20 pct H2SO4+ 30 pct H2O[35] 25 1 min 20
SS316 50 pct H3PO4+ 20 pct H2SO4+ 30 pct H2O[35] 15 1 min 30 s 20
Ti-6Al-4V 700 mL ethyl alcohol+ 300 mL isopropyl alcohol + 60 g AlCl3+ 60 2 min 20
250 g ZnCl2[36]
Inconel 718 600 mL methanol + 330 mL HNO3[37] 18 35 s 20
Hastelloy X 600 mL methanol + 330 mL HNO3[37] 17 40 s 20

C. Dislocation Density dislocations as revealed in Figure 4(a). However, a large


Dislocation density is defined as the number of number of entangled dislocations are observed after grit
dislocations per unit surface area or the total length of blasting as shown in Figure 4(b).
dislocations per unit volume. The methodology for
estimation of dislocation density is already discussed in E. Microhardness
Section II–C. The estimated values of dislocation den-
Figures 5(a) through (f) shows the hardness profiles
sities in different materials are listed in Table VII. It can
of different materials. In all cases, the hardness values
be seen from the table that the range of dislocation
of as-received and annealed samples did not show
densities in different materials in as-received condition is
much variation along the depth. However, after grit
4.34 9 1012 m2 to 5.06 9 1014 m2. Upon annealing,
blasting, higher hardness was identified near the blasted
dislocation density decreased to a range of 5.91 9 1011
surface which gradually decreased with depth to the
m2 to 8.77 9 1013 m2. However, after grit blasting, it
bulk value. The increase in hardness was observed upto
again increased. The range is from 6.31 9 1014 m2 to
a certain depth ranging from around 130 lm to around
3.43 9 1015 m2. The range of dislocation density in
340 lm depending on the material. As observed from
grit-blasted samples is much narrower than that of the
the plots, the depth of hardened layer is low (131 lm)
both as-received and annealed components.
in the case of Ti-6Al-4V and much higher (333 lm) in
the case of low carbon steel. Moreover, it was observed
D. Transmission Electron Microscopy (TEM) Results that the degree of hardening is different for different
Figures 4(a) and (b), respectively, show the TEM materials. For example, the hardness increase is nearly
images of annealed and grit-blasted low carbon steel 80 pct in the case of SS316, whereas it is around 45 pct
specimens. The annealed specimen contained very few in the case of C45 steel. The percentage increases in

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—69


Fig. 1—SEM images of (i) as-received grit-blasted and (ii) annealed grit-blasted surfaces.

hardness of the other materials lie between these two F. X-Ray Diffraction Results
limits. Grazing incidence X-ray diffraction result of
Figure 6 shows the depth profiles of dislocation grit-blasted SS316 revealed a low-intensity martensite
density as well as the microhardness of grit-blasted peak at 2h ~ 44.5 deg. The GI-XRD patterns of
low carbon steel. The dislocation density along the annealed and annealed grit-blasted samples are shown
depth follows a trend similar to that of hardness. in Figure 7(a).The austenite and martensite peaks are

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Table VI. Surface Roughness of the Grit-Blasted Specimens very close to each other and are in overlapped condition.
Moreover, the intensity of the martensite peak is very
Materials Average Surface Roughness (Sa) in lm low as compared to the adjacent austenite peak. So,
Low Carbon Steel these two peaks have been deconvoluted (shown in
As-Received 3.64 ± 0.21 Figure 7(b)) for better understanding. The figure also
Annealed 3.52 ± 0.18 depicts shifting and broadening of both peaks
C45 Steel (Figure 7(a)) after grit blasting. This peak broadening
As-Received 3.50 ± 0.12 indicates an increase in strain and decrease in grain size
Annealed 3.59 ± 0.08 upon grit blasting. The austenite peak at 2h ~ 50.5 deg
SS316 was found to shift towards lower angles in the figure.
As-Received 3.51 ± 0.20 However, shifting of peak at 2h ~ 43.5 deg is not clearly
Annealed 3.69 ± 0.15
visible. Figures 8(a) and (b) show X-ray diffraction
Ti-6Al-4V
As-Received 3.49 ± 0.17 patterns of annealed and grit-blasted low carbon steel.
Annealed 3.63 ± 0.15 The plots confirm shifting and broadening of different
Inconel 718 peaks after grit blasting treatment. It may be noted that
As-Received 3.25 ± 0.09 some reduction in maximum peak intensity was also
Annealed 3.24 ± 0.16 identified after grit blasting.
Hastelloy X
As-Received 2.81 ± 0.11
Annealed 2.73 ± 0.15

Fig. 2—SEM images of (a) alumina grit of 24 mesh size before blasting and (b) eroded alumina grit after blasting.

Fig. 3—Cross-sectional back-scattered electron (BSE) images of low carbon steel (a) before grit blasting and (b) after blasting using alumina
grits.

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Table VII. Dislocation Densities in Different Materials Before and After Grit Blasting

Dislocation Density (m2)

Condition Low Carbon Steel C45 Steel SS316 Ti-6Al-4V Inconel 718 Hastelloy X
12 13 14 14 13
As-Received 4.34 9 10 5.67 9 10 1.11 9 10 5.06 9 10 6.21 9 10 6.16 9 1013
Annealed 5.91 9 1011 5.39 9 1012 8.77 9 1013 1.11 9 1013 2.86 9 1012 4.32 9 1013
Annealed Grit Blasted 6.31 9 1014 7.13 9 1014 2.38 9 1015 3.43 9 1015 1.87 9 1015 2.63 9 1015

Fig. 4—TEM micrographs showing dislocation structures in (a) annealed and (b) annealed grit-blasted low carbon steel specimens at a depth of
50 lm from the surface.

G. Residual Stress parameter (1/Sa) profile was similar to the residual stress
Residual stress depth profiles of the grit-blasted and profile.
non-blasted specimens of different metallic substrates
evaluated by X-ray sin2w technique is shown in
Figures 9(a) through (f). The graphs show that a IV. DISCUSSION
compressive residual stress depending upon the mechan-
ical properties of the materials is induced on the blasted Figure 1 shows rough surfaces having signatures of
surfaces. In each case, the highest residual stress is microcutting and indentation after grit blasting of
recorded slightly below the top surface. This is followed different materials. At a low impingement angle, the
by a steady decrease of compressive stress with depth material is removed from the substrate surface by
and finally become tensile. microcutting and ploughing.[38] On the other hand, the
primary mode of material removal is indentation and
extrusion at an impact angle of 90 deg. Repeated impact
H. Roughness Variation After Electropolishing of the abrasive grits on the surface leads to the
An interesting observation was made after removing formation of platelets (shown by rectangles in
successive layers from the grit-blasted samples by Figure 1) with extruded materials at the periphery.
electropolishing. Figure 10 shows the variation of However, prolonged impact of the abrasive particles
inverse of the roughness of electropolished surface (1/ eventually leads to erosion of the extruded material
Sa) with depth for the annealed grit-blasted low carbon from the surface.[39] Although the present study was
steel specimen. The residual stress is also plotted in the undertaken at a nominal impingement angle of 90 deg,
same figure. The as-grit-blasted sample had a high both mechanisms, namely, indentation and microcut-
roughness value (Sa = 3.52 ± 0.18 lm). The roughness ting, were found to be active concurrently. This is
of the electropolished surfaces was found to decrease attributed to the motion characteristics of the abrasive
with depth, and finally, a steady roughness value was particles entrained in the air jet during grit blasting. In
obtained. In other words, the inverse of the roughness addition to translation, the abrasive particles undergo

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Fig. 5—Hardness depth profiles of as-received, annealed and grit-blasted (a) low carbon steel, (b) C45 steel, (c) SS316, (d) Ti-6Al-4V, (e) Inconel
718 and (f) Hastelloy X substrates. Note The abbreviations used in the plots are designated as follows: AR as-received, AN annealed, AR_GB
as-received grit blasted, AN_GB annealed grit blasted.

rotation while coming out of the nozzle. This rotational The grit materials also demonstrated signatures of
component can influence the effective impact angles of surface damage. Upon collision with the substrate, the
individual abrasive grits[40] bringing about both micro- sharp edges of the grits are broken. Moreover, the
cutting and indentation. incoming abrasive particles from the nozzle collide with

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—73


the ricocheting particles from the target surface. This
leads to grit fragmentation. Progressive grit damage
during the blasting process is evident from Figure 2.
Figure 3 shows evidence of plastic deformation of the
target surface (annealed low carbon steel) upon grit
blasting. During blasting, the abrasive particles impinge
on the substrate surface at high a velocity and apply a
large amount of stress on the substrate surface. The
applied stress, in turn, moves the pre-existing disloca-
tions by slip and twining. Plastic deformation results
from the cumulative motion of a number of dislocations.
At the same time, new dislocations are generated and
multiplied from pre-existing dislocations, defects, and
grain boundaries through Frank-Reed mechanism.[41]
Hence, the dislocation density is increased after grit
blasting (Table VII). It may be noted that a moderately
high dislocation density was found in the as-received
Fig. 6—Dislocation density and microhardness variation along the samples. Upon annealing, the dislocation density was
depth of annealed grit-blasted low carbon steel.
found to reduce to an extent. This is attributed to the

Fig. 7—Grazing incidence X-ray diffraction pattern of SS316 with an incidence angle of 1 deg and 0.03 deg step size (a) annealed and annealed
grit-blasted samples, (b) deconvoluted peaks of austenite and martensite in the 2h range of 41 to 47 deg.

Fig. 8—(a) X-ray diffraction patterns of annealed and grit-blasted low carbon steel substrates, (b) magnified view of (3 1 0) peak in the 2h range
of 113 to 120 deg.

74—VOLUME 52A, JANUARY 2021 METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 9—Residual stress depth profiles of as-received, annealed and grit-blasted specimens of (a) low carbon steel, (b) C45 steel, (c) SS316, (d)
Ti-6Al-4V, (e) Inconel 718 and (f) Hastelloy X.

absorption of dislocations at grain boundaries during Figure 4(b) also reveals the region showing disloca-
recovery stage.[42] Figure 4(a) shows a TEM micrograph tion interaction and entanglement (shown using an
of annealed low carbon steel specimen indicating low ellipse) in grit-blasted low carbon steel substrate. Dis-
dislocation density. A high density of dislocations in the location entanglement occurs during dislocation move-
grit-blasted sample is observed in Figure 4(b). ment at intersecting slip planes. At that instant, higher

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—75


stress is required for further slip to occur.[43] Under this
circumstance, the material is said to have undergone
strain hardening.
Figure 5 shows the hardness depth profiles of differ-
ent materials. In all cases, the hardness is highest near
the grit-blasted surface. With increase in depth, the
hardness gradually decreases and finally attains a steady
value which is equal to the material hardness in
as-received or annealed condition. The depth to which
the hardness is higher than that of the annealed material
is the affected layer. The depth of the affected layer and
percentage increase in hardness vary with the material
properties. The properties of the materials, e.g., yield
strength, strain hardening exponent, and so on, along
with the depth of affected layer, maximum compressive
residual stress, and percentage increase in hardness (AR
to AR_GB, AN to AN_GB and average) of different
Fig. 10—Variation of the inverse of the roughness parameter (1/Sa) materials under consideration are listed in Table VIII.
and residual stress with depth. The measurements were made on Figure 6 shows the dislocation density variation along
annealed grit-blasted low carbon steel specimen.
the depth of annealed grit-blasted low carbon steel

Table VIII. The Values of Yield Strength, Strain Hardening Exponent, Depth of Affected Layer, Maximum Compressive Residual
Stress, and Percentage Increase in Hardness of the Materials Under Investigation

Increase in Hardness ( pct)


Yield Depth of
Strength Strain Hardening Affected Layer Maximum Compressive AR to AN to
Materials (MPa) Exponent (n) (lm) Residual Stress (MPa) AR_GB AN_GB Average
Low Car- 250 0.643[44] 333 ± 5.5 340 ± 3 72.45 71.69 72.07 ± 1.5
bon
Steel
C45 Steel 370 0.25[45] 281 ± 10 382 ± 7 44.41 42.36 43.34 ± 1.07
SS316 290 0.8722[46] 293 ± 2.5 639 ± 21 79.78 80.89 80.34 ± 0.85
Ti-6Al-4V 880 0.5387[47] 131 ± 7 693 ± 12 49.56 51.38 50.47 ± 0.91
Inconel 725 0.6828[48] 263 ± 2 774 ± 33 64.59 62.81 63.7 ± 0.89
718
Hastelloy 380 0.55[49] 230 ± 5.5 660 ± 48 62.42 59.81 61.11 ± 1.3
X

Fig. 11—Correlation between (a) depth of the affected layer and yield strength and (b) percentage increase in hardness and strain hardening
exponent.

76—VOLUME 52A, JANUARY 2021 METALLURGICAL AND MATERIALS TRANSACTIONS A


Table IX. Calculated Texture Coefficient of Annealed and Annealed Grit-Blasted Low Carbon Steel Substrate

Texture Coefficient (Tc)

Condition (1 1 0) (2 0 0) (2 1 1) (2 2 0) (3 1 0) (2 2 2)
Annealed (AN) 1.538 0.703 0.672 1.142 1.144 0.798
Annealed Grit Blasted (AN_GB) 1.458 0.738 1.128 1.008 1.008 0.642

specimen. The microhardness profile has also been accomplished by analyzing peak shifting and broaden-
shown in the same plot. The dislocation density profile ing. Figures 7 and 8 show the evidence of shifting and
follows a similar trend as that of the hardness with the broadening of X-ray diffraction peaks after grit blasting
specimen depth. The top layer receives the impinging of low carbon steel substrate. A reduction in maximum
abradants during grit blasting. Hence, the top layer peak intensities of the diffraction peaks was also
harbors a high dislocation density. The effect of impact, observed after grit blasting. This is attributed to the
i.e., the degree of deformation, reduces with depth. roughening of the substrate surface after repeated
Hence, the dislocation density reduces with the depth of abrasive grit impacts. Moreover, there is a possibility
the grit-blasted specimen. The extremely work-hardened of crystallographic texture generation after plastic
top layer also has a high hardness. The degree of work deformation in grit-blasted material. This may lead to
hardening reduces with the depth and so does the a change in the integrated intensity as well.[53,54]
hardness. Preferential growth of some particular plane is observed
Figure 11(a) shows depth of affected layer vs yield in the grit-blasted material. This is assessed by calcula-
strength plot of various materials. The affected layer tion of texture coefficient values of the crystallographic
depth tends to vary with the yield strength in a planes in a material. The texture coefficient (Tc) of a
somewhat linear fashion. Ti-6Al-4V with its higher yield crystallographic plane (h k l) is calculated using the
strength has a thinner affected layer. On the other hand, following equation[32]:
low carbon steel, with its lower yield strength, offers a 
much thicker affected layer (Table VIII). Therefore, it IðhklÞ IoðhklÞ
TcðhklÞ ¼ hP  i ½4
can be concluded that the yield strength of the materials 1=N N
1 IðhklÞ IoðhklÞ
significantly influences the depth of affected layer in grit
blasting. On the other hand, the increase in hardness of where I(h k l) and Io(h k l) are the measured and relative
different materials relies on the ability of the materials to intensity of the corresponding lattice plane, and N is the
work harden. The strain hardening exponent (n) is a number of reflections. The calculated texture coefficients
measure of work or strain hardening behavior of for annealed (AN) and annealed grit blasted (AN_GB)
materials. Larger the value of strain hardening expo- for low carbon steel specimen are listed in Table IX. An
nent, higher would be the hardening for a given plastic increase in the Tc value for (2 0 0) and (2 1 1) planes in
strain.[50] A linear correlation was found between the the grit-blasted specimen is observed from the table.
percentage increase in hardness after grit blasting and Therefore, it can be said that these planes grow
the strain hardening exponents of the materials, as preferentially as compared to the other planes owing
plotted in Figure 11(b). The increase in subsurface to severe plastic deformation during grit blasting
hardness is maximum (80 pct) for SS316 with a strain process.
hardening exponent of n =0.8722,[46] whereas, in the The peak broadening is affected by various factors,
case of C45 steel (n = 0.25,[45] only 43 pct hardness e.g., grain size, strain, and broadening owing to instru-
increase was observed. mental errors.[55] This peak broadening and conse-
Grit blasting of SS316 resulted in a phase transfor- quently the plastic deformation after grit blasting can
mation from austenite to martensite as indicated in be assessed by observing full width at half maximum
Figure 7. This phase change is attributed to severe (FWHM) of a particular X-ray diffraction peak of a
plastic deformation owing to grit blasting.[51] The material. FWHM values of the same peak used for stress
estimated X-ray penetration depth of Cu-Ka radiation measurement of different materials are plotted against
at 1 deg incidence angle is nearly 240 nm. Therefore, it depth as shown in Figures 12(a) through (f). The
may be assumed that the martensite is induced very near averages of FWHM values of eleven peaks correspond-
to the blasted surface. Multigner et al.[52] also identified ing to each stage tilt angles are presented along with an
deformation-induced a martensite in Al2O3 and ZrO2- error bar. The FWHM values of the grit-blasted samples
blasted 316 LVM steel. They, however, described the were found to be higher as compared to the non-treated
formation of martensite inside a thinner severely samples. Moreover, the FWHM values gradually
deformed layer (less than 100 nm) using less energetic decrease with depth and finally reduce to that of the
Co radiation. annealed sample. This indicates that the deformation is
As expected, residual stress is also induced on the maximum at the blasted surface and decreases with the
blasted surface owing to plastic deformation. The depth.
measurement of residual stress using XRD is

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—77


Fig. 12—Variation of FWHM with depth of as-received annealed and grit-blasted (a) low carbon steel, (b) C45 steel, (c) SS316, (d) Ti-6Al-4V,
(e) Inconel 718 and (f) Hastelloy X substrates.

Figure 9 shows the residual stress depth profiles of underlying material restricts that plastic flow, and hence,
different substrate materials. A compressive residual a compressive stress is induced at the blasted surface.
stress field with a maximum value at a certain depth was However, the deformation on the blasted top surface is
induced after grit blasting. During grit blasting, the restricted only by the underlying material but the
impacted grits try to make the material flow outwards material at a certain depth is hindered by both top
by deforming the work material plastically. The and bottom layer of material. Moreover, stress

78—VOLUME 52A, JANUARY 2021 METALLURGICAL AND MATERIALS TRANSACTIONS A


relaxation may occur at the free surface. Thus, the The total effective strain and strain rate are assumed
maximum stress is attained at a certain depth of the to be 0.4 and 100,000/s, respectively, in shot peening
material instead of the top surface. process that is similar to grit blasting.[58,59] Neglecting
The residual stress profiles are similar to the stress the temperature in case of blasting and substituting the
profile obtained in shot peening process.[56,57] The strain and strain rate values in Eqs. [6] through [11], the
residual stress is induced to a certain depth inside the flow stress values of the materials under high strain and
material. This depth is termed as the plastically influ- strain rate were calculated and plotted against maximum
enced depth.[58] Similar to the hardness profiles compressive residual stress in Figure 13. The plot clearly
(Figure 5), a lower depth of affected layer was achieved shows a linear correlation between the magnitude of
in the case of Ti-6Al-4V as compared to other materials maximum induced stress and Johnson–Cook flow stress.
(Figure 8(d)).The thicknesses of the affected layers given It shows that higher is the stress required for a material
in Figure 5 (hardness) are in agreement with those in to flow plastically as predicted by Johnson–Cook model,
Figure 12 (FWHM) and Figure 9 (residual stress). higher is the induced maximum compressive stress upon
The grit blasting-induced maximum compressive grit blasting.
residual stresses are found to be different for different The strain and strain rate are high near the free
materials. Low carbon steel possessed the lowest value surface where the actual material flow occurs. Hence,
of maximum compressive stress while Inconel 718 the maximum compressive residual stress could be
possessed the highest value. The maximum stress correlated to the Johnson–Cook flow stress
obtained is influenced by several factors such as yield (Figure 13). On the other hand, the depth of affected
strength, strain hardening modulus, strain hardening layer merely indicates to what depth the material has
exponent, strain rate sensitivity factor, and so on. This is undergone yielding. Hence, the depth of affected layer is
elucidated by Johnson–Cook strength model.[47,48] The well correlated to the yield strength of the materials
model is used to represent the strength behavior of (Figure 11(a)).
metals, subjected to high strains, strain rates, and Figure 10 shows the variation of the roughness of
temperatures. With this model, the yield stress varies electropolished surface and residual stress with depth.
depending on strain, strain rate, and temperature. The Grit-blasted surface was rough with a maximum peak to
model defines the flow or yield stress r as follows: valley height (Sz) of around 40 lm. Therefore, after
removing 40 lm, the roughness of the exposed (to acid)
r ¼ ½A þ Ben ½1 þ C ln e_  ½1  T m  ½5 surface is expected to attain a stable value. However, in
where e is the effective plastic strain, e_  is the normalized this case, the roughness decreased to a depth of around
effective plastic strain rate, T is the Homologous 225 lm and finally achieved a stable value. This is
temperature ¼ ðT  Troom Þ=ðTmelt  Troom Þ, A is yield attributed to the difference in dissolution rates of the
strength, B is the strain hardening modulus, C is strain different phases of the material under residual stress.
rate sensitivity factor, n is strain hardening exponent, The low carbon steel coupon consists of two phases,
and m is thermal softening coefficient. namely, ferrite and pearlite (Figure 3). These two phases
According to this model, the flow stresses of the dissolve at different rates during electropolishing, espe-
considered materials are as follows: For low carbon cially when the specimen is subjected to a stress. Salamci
steel,[44] et al.[60] investigated the corrosion behavior of plain
carbon steels of different phases obtained using different
rðMPaÞ ¼ 217 þ 234e0:643 ½1 þ 0:076 ln e_   ½6 cooling rates. It was found that the rates of dissolution
changes with the phase content of the material. At a
For C45 steel,[45]
h i
rðMPaÞ ¼ 546 þ 487e0:25 ½1 þ 0:015 ln e_   1  T 1:22
½7
For SS316,[46]
h i
rðMPaÞ ¼ 388 þ 1901e0:8722 ½1 þ 0:02494 ln e_   1  T0:6567 ½8

For Ti-6Al-4V,[47]
h i
rðMPaÞ ¼ 980:8 þ 732:16e0:5387 ½1 þ 0:01829 ln e_   1  T0:834 ½9

For Inconel 718,[48]


h i
rðMPaÞ ¼ 1132 þ 1091e0:6828 ½1 þ 0:0147 ln e_   1  T1:3225 ½10

For Hastelloy X,[49]


rðMPaÞ ¼ 380 þ 1200e0:55 ½1 þ 0:012 ln e_   ½11
Fig. 13—Correlation between maximum induced stress and flow
stress calculated from the Johnson–Cook model.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 52A, JANUARY 2021—79


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