Original Article

Proc IMechE Part C:

J Mechanical Engineering Science
Performance Study of Cryo-Treated 0(0) 1–17
! IMechE 2021
End Mill Via Wet, Cryogenic, and Article reuse guidelines:
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Hybrid Lubri-Coolant-Milling DOI: 10.1177/09544062211017160
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Induced Surface Integrity of

Biocompatible Mg Alloy AZ91D

Rahul Davis and Abhishek Singh

Abstract
The excellent biodegradability of the magnesium (Mg) alloys is gradually proving them as the potential substitutes to
several biomedical implants such as chemotherapy ports or screws, which are required to be removed via secondary
surgeries after a specific period of time. However, an early degradation of these alloys even before the complete healing
of the damaged tissue, when exposed to the physiological atmosphere, has been limiting their full-fledged application.
Some latest research articles suggest that such challenges can be effectively overcome by improving the surface integrity
of Mg alloys using the sustainable manufacturing techniques, such as cryogenic machining. Recent literatures also report
the outperformance of the cryogenically treated (cryo-treated) cutting tools for achieving an enhanced surface integrity.
In this relation, the present research attempts to improve the surface integrity of one of the most commonly used
biocompatible alloys of magnesium, known as AZ91D. For this reason, a TiAlN coated-cemented carbide end mill was
used in an untreated and cryo-treated state amid wet, cryogenic, and hybrid-lubri-coolant-milling conditions. The milling
and FESEM (field emission scanning electron microscopy) results showed a considerable improvement in the surface
integrity in terms of an augmented surface roughness and microhardness at 56.52 m/min cutting speed with the cryo-
treated end mill during hybrid-lubri-coolant-milling. At the high cutting speed hybrid-lubri-coolant-milling, the cryo-
treated end mill attained 35.71% and 48.07% better surface finish than that of cryo and wet-lubri-coolant-milling,
respectively. Although, the highest surface microhardness was achieved by the cryo-treated end mill amid cryo-lubri-
coolant-milling, due to the poorest surface quality observed in terms of the maximum number of machining-induced
cracks, the hybrid-lubri-coolant-milled surface was preferred over the cryo and wet-lubri-coolant-milled surfaces.
Further, the FESEM and EDS (energy-dispersive X-ray spectroscopy) analyses confirmed the oxide layer produced by
the cryo-treated end mill amid hybrid-lubri-coolant-milling, to be the thinnest (12.16 mm) and most uniform passivation
layer.

Keywords
Magnesium alloy AZ91D, wet, cryogenic, and hybrid-lubri-coolant-milling, untreated and cryo-treated end mill, surface
roughness, microhardness, end mill wear
Date received: 5 December 2020; accepted: 21 April 2021

Introduction on the permanent and temporary basis, are called the

Each day a large number of human bone or tissue
fracture cases are dealt by the medical practitioners
across the globe. Generally, the plausible reasons of
such cases are sport injuries, falls, and vehicle acci-
dents. Curing of these damages or fractures can be
effectively performed by placing some biomedical
devices, also known as implants, either inside or on
the body surface. The biomedical devices, replacing
the lost body parts or supporting the damaged ones
non-degradable and degradable implants, respective-
ly. Heart pacemaker, cardioverter defibrillators,
Department of Mechanical Engineering, National Institute of
Technology Patna, Patna, India
Corresponding author:
Rahul Davis, Department of Mechanical Engineering, National Institute
of Technology Patna, Patna 800005, India.
Email: rahul.me18@nitp.ac.in
2 Proc IMechE Part C: J Mechanical Engineering Science 0(0)
intra-uterine device (IUD), dental and orthopedic
devices, spine screws, rods, and discs are some of
the examples of non-degradable and degradable
implants.1 In the case of the non-degradable metallic
implants, if their Young’s modulus is comparatively
high (100–200 GPa) then their high stiffness may
adversely affect the density of the fractured bone
(10–45 GPa).2 Therefore, in some cases, the non-
degradable implants such as surgical meshes, screws,
plates, and nails, are recommended to be removed
after a predetermined period of time. However, the
removal of an implanted device may accompany the
risk of failure, infection, and skin contamination.1
Hence, such uncertainties motivated the researchers
to invent some competent alternatives, also known
as the degradable implants, to avoid the risks associ-
ated with secondary surgeries. In this relation, the
researchers have recommended the magnesium
alloys as the more suitable degradable implant mate-
rials over the synthetic biodegradable polymers (such
as polylactide and polydioxanone) owing to their ade-
quate degradability in the presence of human body
fluid.3 Mg alloys not only exhibit the satisfactory bio-
compatibility and osteoconductivity, but also a den-
sity (1.75–18.5 g/cm2) and Young’s modulus (40–
45 GPa) which are awfully close to the human bone
density (1.8–2.1 g/cm2) and Young’s modulus (10–
27 GPa), respectively.4 Moreover, the magnesium
implants are capable of comparatively quick bone
development and its cell stimulation, when alloyed
with Sr, Cu, Ag, and Ca.5 Despite all such remarkable
properties, the surgeons have faced challenges in
terms of the early degradation of magnesium implants
in some cases, which resulted in an incomplete recov-
ery of the fractured bone or tissue. Therefore, surface
coating, metal alloying, corrosion resistant layer, and
mechanical techniques were proposed by Uddin et al.6
to delay the abrupt deterioration of the Mg implants
by enhancing their surface integrity. In this regard, a
substantial improvement in the surface integrity of
Mg-based alloys at a relatively low cost and quick
manner was noticed via mechanical means.
However, the finally achieved surface, metallurgical,
and mechanical properties primarily depend on the
type of material subtractive method and cutting tool
behavior.7 In addition, in all the CNC assisted sub-
tractive processes, the cutting tool performance is fur-
ther subjected to the variations in the input control
variables such as feed rate, cutting or spindle speed,
depth of cut, machining pressure, frictional force,
lubri-coolant condition, and generated enormous
heat. The detrimental influence of any such alteration
can weaken and disintegrate the cutting ability of the
cutting tool, and thus, induce the tool wear.8 Therefore,
considerable efforts have been made in this regard
towards improving the cutting tool performance by
guarding it against wear with the assistance of surface
coating and heat and cryogenic treatments. Cryogenic
treatment can substantially enhance the mechanical
toughness and wear in addition to chemical, thermal,
electrical, and metallurgical properties of the cryo-
treated cutting tool.9,10 Besides, several studies noticed
the carbide spread in a homogenous fashion on the
surfaces of the cryo-treated specimens.9,11–13
Therefore, some comparative investigations associated
with CNC machining also reported the enhanced func-
tionality of the cryo-treated cutting tools over
untreated ones.13,14 Apart from this, the lubri-coolant
conditions also influence a subtractive process signifi-
cantly. Dhar and M. Kamruzzaman11 found that the
wet environment of machining significantly enhanced
the tool life of cryo-treated cutting tool, which was
38.6% longer compared to dry environment. In this
series, in recent years, the application of liquid nitrogen
(LN2), as an efficient and environment-friendly cool-
ant, has become exceedingly popular. A few studies
reported that LN2 can not only dissipate the excessive
heat from the cutting zone but can also achieve the
higher degree of precision and surface integrity,
longer fatigue and cutting tool life, and higher material
removal rate compared to other lubri-coolant strate-
gies.15,16 However, a study also noticed a lesser cutting
force in the presence of hybrid cooling (cryogenic and
minimum quantity lubrication) compared to cryogenic
and wet lubri-coolants.17 Davis and Singh18 used wet,
cryogenic, and hybrid (LN2þwet) machining environ-
ments with the untreated and cryo-treated end mills
during the end milling of Mg alloy AZ31B. Further,
the improved surface integrities were observed with the
combinations of cryogenic machining with untreated
end mill and hybrid machining with cryo-treated end
mill. The study also reported the formation of a pas-
sivation layer suggesting an enhanced biocompatibility
of the hybrid-milled surface produced by the cryo-
treated end mill.
The availability of limited studies on the CNC
machining of biocompatible magnesium alloys with
the assistance of different lubri-coolant strategies
and cryo-treated cutting tools, towards the improve-
ment of surface integrity for the biomedical implant
applications, have motivated the present research. In
the light of the above, this research has found an
opportunity to obtain a few adequate combinations
of lubri-coolant-milling conditions (wet, cryogenic,
and hybrid) and cutting tools (in an untreated and
cryo-treated state) to achieve an improved surface
integrity on the end milled biocompatible Mg alloy
AZ91D.
Materials and methods
A comprehensive review stated that the a and b-phase
of Mg alloy AZ91D enables it to exhibit excellent
mechanical strength, corrosion resistance, and
osteoblastic conductivity, which are highly desirable
properties for potential biomedical implant
manufacturing.19 Such appealing properties of this
alloy of magnesium inspired the present research to
Davis and Singh
Table 1. Major constituents present in Mg alloy AZ91D specimen.
Al (%) Mn (%) Zn (%) Si (%)
8.8 0.18 0.41 0.1
Figure 1. The cycle of deep cryogenic treatment of the end mill.
consider it to be the workpiece material. The work-
piece specimens of Mg alloy AZ91D consisting of the
following composition (as outlined in Table 1), were
procured from Petromet Flange Inc., Mumbai, India.
Experimental setup
The poor surface integrity of a mechanically proc-
essed degradable material can lead to a local crack
initiation and consequently, to corrosion, and thus,
to faster degradation. Moreover, the high flammabil-
ity of magnesium alloys additionally contributes
towards the low quality of surface finish by causing
flame ignition and flank built up amid dry machining.
Therefore, to overcome such challenges, some
researchers have strongly recommended the use of
optimal settings of the input control variables such
as cutting speed, feed rate, and depth of cut, in addi-
tion to the incorporation of an effective cooling
medium in the machining zone (at cutting tool-
workpiece and cutting tool-chip interface) during
machining of the magnesium alloys.2,20
The present research experimentation was con-
ducted on a 3-axis CNC XL Mill with variation in
cutting speed (m/min), feed rate (mm/rev), and depth
of cut (mm) upto two levels. An aluminium titanium
nitride (Ti-NAMITE) coated end mill (Model:
Kyocera 48,509 solid carbide/4 Flute, SER 01S)
with 3700 HV hardness, 1100  C thermal stability,
40 mm length, and 6 mm diameter, was chosen to be
the cutting tool for the present work.
3
Cu (%) Fe (%) Ni (%) Mg (%)
0.02 0.003 0.002 Remainder
On the basis of a recently published article consist-
ing of a significant role of a cryo-treated end mill
during the milling of Mg Alloy AZ31B in different
machining environments,18 the current study also
aims to assess the performance of a cryo-treated end
mill in different lubri-coolant-milling conditions.
A few studies reported that as a result of the cryo-
genic treatment of solid carbide, the particle size of a,
b, and g-phase were found to be improved, which
could further segregate the carbide grains, improve
hardness, toughness, and flank, abrasive, and nose
wear. However, the cryogenic treatment may adverse-
ly affect the brittleness of the solid carbide, which
may lead to the tool failure.21 In the present cryogenic
treatment, in order to save the end mill against the
thermal impact (due to an abrupt subjection to the
cryogenic environment) and to exhibit an improved
carbide distribution in the microstructure, the end
mill was preferred to be gradually deep cryo-treated
(for 24 hours) at 1  C rate of cooling in the atmo-
sphere of the most environment-friendly cryogenic
liquid nitrogen (LN2).8,22 In this relation, Figure 1
demonstrates the deep cryogenic treatment (DCT)
cycle consisting of four basic periods or phases that
the end mill goes through to be transformed into a
cryo-treated end mill. Figure 2 shows a schematic dia-
gram of the basic machining setup demonstrating wet,
cryo, and hybrid-lubri-coolant-milling. The wet-lubri-
coolant-milling consisted the application of the con-
ventional cutting oil and the cryo-lubri-coolant-
milling employed the use of liquid nitrogen (LN2),
4 Proc IMechE Part C: J Mechanical Engineering Science 0(0)
Figure 2. Schematic diagram of the milling set up presenting the cryo, wet, and hybrid-lubri-coolant-milling conditions.
Table 2. Input control variables and their levels.
Variable Level
Cutting speed (m/min) 28.26
Feed rate (mm/rev) 0.40
Depth of cut (mm) 0.80
whereas the hybrid lubri-coolant-milling combined
the wet and cryo-lubri-coolant-milling conditions.
GeminiSEM 500-Zeiss Field-emission scanning elec-
tron microscope (FESEM) was used for analysing the
surfaces milled under all the lubri-coolant-milling
conditions.
Experimental methodology
This work employed the one-factor-at-a-time
(OFAT) methodology for designing the experiments.
The OFAT approach can achieve an improved out-
come with higher accuracy compared to many other
design of experiment (DOE) approaches. Table 2
presents the various input control variables and
their levels used in this research. According to
OFAT methodology, each of the shown variable
was varied upto two levels at a time, while keeping
the other two variables as constants for all the three
wet, cryo, and hybrid-lubri-coolant-milling condi-
tions. Moreover, in order to notice the actual influ-
ence of cryogenic treatment on the performance of the
cryo-treated end mill, a separate set of similar experi-
ments was conducted with an untreated end mill, fol-
lowed by the comparison of the observations
obtained with both untreated and cryo-treated end
mill.
Response milling characteristics
56.52
0.60 Surface roughness, topography, microhardness, resid-
1.50 ual stress, phase transformation, and corrosion resis-
tance are some of the major machining-induced
surface integrity characteristics.23,24 In the case of
the magnesium alloys, their corrosivity and instability
can considerably increase with a substantial rise in
surface roughness and reduction in surface micro-
hardness, respectively, which further leads to a com-
paratively quick degradation.25 However, this surface
integrity can be substantially regulated by achieving
the desired surface finish and microhardness, since an
improved finish can result into an enhanced corrosion
resistance and an improved microhardness into the
enhanced stability, host tissue maturation and
mechanical resistance.26 Therefore, in the present
work, out of all the above-mentioned surface integrity
characteristics, surface roughness (mm) and micro-
hardness (HV) were chosen to ascertain the surface
integrity of the milled surface of Mg alloy AZ91D.
Precise/TR110 Plus Surface Roughness tester was
employed to assess the roughness and Blue Star Ltd./
BSHT-FHV1-50 Vickers Hardness tester was used to
determine the microhardness of all the surfaces
machined under different lubri-coolant conditions.
The surface roughness was measured by moving
the tester probe over a sampling dimension of
1.5 mm on the machined region. On the other hand,
the surface microhardness was measured by pressing
Davis and Singh
the diamond indenter with 100 gf load into the
machined surface for 10 seconds and estimating the
diagonal dimensions of the obtained impression. A
minimum of three trials were conducted for measur-
ing both surface roughness and microhardness.
Results and discussion
The following segments present the findings observed
after the successful completion of each experimental
run followed by a detailed discussion with the assis-
tance of graphical and pictorial studies:
Analysis of the milling-induced surface integrity
characteristics
Figure 3(a) and (b) present the variation in the surface
roughness of Mg alloy AZ91D specimens machined
amid wet, cryo, and hybrid-lubri-coolant-milling con-
ditions with the application of untreated and cryo-
Figure 3. Surface roughness obtained with the (a) untreated and (b) cryo-treated end mill; Surface microhardness obtained with the
(c) untreated and (d) cryo-treated end mill.
5
treated end mill, respectively. Similarly, Figure 3(c)
and (d) show the variation in microhardness of the
same in identical lubri-coolant-milling conditions
with the use of untreated and cryo-treated end mill,
respectively.
It is evident in Figure 3(a) and (c) that at 56.52 m/
min cutting speed, the untreated end mill attained the
lowest value of surface roughness and highest value of
microhardness amid the cryo-lubri-coolant-milling,
followed by the hybrid and wet-lubri-coolant-milling.
The plausible reason lies in the fact that the cryo-
lubri-coolant-milling can substantially reduce the
smearing and plucking mechanism.27 The least stan-
dard deviation during cryo-lubri-coolant milling con-
firmed the uniformity of surface roughness and
microhardness (improved surface integrity) at different
sites on the cryo-lubri-coolant-milled milled surface.
However, the untreated end mill achieved a relatively
high surface roughness and low microhardness at the
small levels of depth of cut (0.8 mm) and feed rate
6 Proc IMechE Part C: J Mechanical Engineering Science 0(0)
(0.40 mm/rev) during hybrid, followed by wet-lubri-
coolant milling.
According to the Figure 3(b) and (d), the cryo-
treated end mill achieved the lowest surface rough-
ness and highest surface microhardness at at 56.52 m/
min cutting speed during hybrid-lubri-coolant mill-
ing, followed by cryo and wet-lubri-coolant milling.
The least standard deviation represents the uniformi-
ty of surface roughness and microhardness (improved
surface integrity) at different sites on the hybrid-lubri-
coolant-milled surface. However, the cryo-treated end
mill achieved a moderately high surface roughness
and low surface microhardness at the small levels of
depth of cut (0.8 mm) and feed rate (0.40 mm/rev)
during wet, followed by cryo-lubri-coolant milling.
Moreover, it was noticed in Figure 3(b) and (d)
that in wet-lubri-coolant-milling and at high cutting
speed, the cryo-treated end mill achieved better sur-
face roughness and microhardness compared to the
untreated one. The credible cause of the same is an
improved heat dissipation during the milling process
due to an enhanced thermal conductivity of the cryo-
treated end mill. However, the cryo-treated end mill
Figure 4. Surface milled at 56.52 m/min cutting speed with the untreated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
displayed its worse performance in the case of cryo-
lubri-coolant milling.
Generally, in the case of the TiAlN coated cutting
tools, the Al content leads to the formation of com-
posite ceramic Al2O3 layer during the high heat gener-
ation, which further minimizes the adverse
consequences of oxidation and thus, protects the tool
cutting edge against quick wear, plastic deformation,
and chipping.28,29 A study reported that DCT can sub-
stantially strengthen the TiAlN coating present on the
cutting tools by improving surface hot hardness, ther-
mal conductivity, uniformity of carbide distribution,
and interfacial adhesion bonding.30 However, some
factors such as the specific DCT soaking temperature,
in addition to the intermittent loading by the chips on
the cutting edge and large recurring thermal and
mechanical stresses, lead to the minimization of Al
content in the coating layer, and thus, can also
weaken the adhering strength of Ti-NAMITE coat-
ing.30,31 Hence, the possible reason of obtaining the
poor surface roughness and microhardness with cryo-
treated end mill during both cryo and hybrid-lubri-
coolant-milling, might be the weaker adhering strength
Davis and Singh
of Ti-NAMITE coating as a result of the factors men-
tioned above.31 Therefore, those specific locations on
the cutting edge that lose the coating, are more prone
to cutting forces and wear, and thus, produce rough
surface, when come in contact with the workpiece.
Moreover, the degraded coating particles, clogged
between the cutting edge and workpiece surface,
might also contribute towards the poor finish and
microhardness on the milled surfaces. This can further
result in a significantly increased brittleness of the end
mill after cryogenic treatment and also during the low
temperature lubri-coolant-milling conditions. Such a
rise in the brittleness leads to the damage the of the
cutting tool especially when used at higher levels of the
cutting speed, feed rate, and depth of cut.13,23 Similar
observations were noticed by a previous research arti-
cle.32 In the case of both untreated as well as cryo-
treated end mill, the high level of cutting speed accom-
panies lesser cutting force and built-up edge compared
to the high levels of feed rate and depth of cut, and
thus, acquires the minimum surface roughness and
maximum surface microhardness. These findings are
found in strong agreement with the previously estab-
lished conclusions of a research article.10
Figure 5. Surface milled at 0.60 mm/rev feed rate with the untreated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
7
The improved surface microhardness was noticed
in those cases (Figure 3(c) and (d)) where a compar-
atively low temperature milling atmosphere was pre-
sent. Although the results differed because of the end
mill treatment conditions, the major reason behind
such a rise in microhardness lies in the fact that the
low temperatures induce strain hardening and grain
refinement in the surface being machined and sub-
stantially lower down the thermal softening and
high temperature in the milling zone.33 Hence, in
Figure 3(c), cryo-lubri-coolant-milled surfaces with
the untreated end mill were observed with the highest
microhardness, followed by hybrid and wet-lubri-
coolant-milled surfaces. However, as explained
above in the case of the cryo-treated end mill
(Figure 3(d)), the end mill fails to perform satisfacto-
rily in the low temperature lubri-coolant-milling con-
ditions due to the development of micro cracks at
high cutting speed and increase in the chances of
tool breakage at the high feed rate and depth of
cut.13,23 Therefore, such damaged machined surfaces
exhibit the high values of roughness and thus, poor
surface microhardness. The standard deviation in sur-
face roughness as well as microhardness was noticed
8 Proc IMechE Part C: J Mechanical Engineering Science 0(0)
to be the most in all the three cases of wet, cryo, and
hybrid-lubri-coolant milling at high feed rate
(0.60 mm/rev), which depicts that the largest amount
of variation in the surface integrity was caused by the
high feed rate followed by depth of cut. The possible
reason of observing the highest surface roughness
value in the case of high feed rate level is the ineffi-
ciency of proper removal of excess material from the
machined surface as cutting force rises.
Microscopic study of the specific wet, cryo, and
hybrid-lubri-coolant-milled surfaces
Several recent investigations reported the negative
impact of poor surface finish and microhardness, cor-
rosive lubri-coolant machining conditions, induced
residual stress, and tensile stress in the form of the
stress corrosion cracking (SCC) developed on the
machined surfaces during the traditional machining
of magnesium alloys.18,34,35 Therefore, the present
study has incorporated the following segments
which deal with the examination of the surfaces
observed with the highest and the lowest surface
integrities in addition to SCC as a result of milling
with both untreated and cryo-treated end mills during
Figure 6. Surface milled at 1.5 mm depth of cut with the untreated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
all the lubri-coolant-milling conditions. For this
reason, FESEM analysis of all the milled surfaced
of interest was conducted and the presence of the
stress-induced cracks at specific locations, was pri-
marily displayed. In addition, some poorly milled
regions (carrying feed marks, impressions, and
scratches) and accumulated chips on the milled surfa-
ces, were also pointed.
Examination of surfaces milled with untreated end mill. In
Figure 4, on the basis of a general visual inspection
via FESEM, the surface milled by the untreated end
mill at 56.52 m/min cutting speed in cryo-lubri-
coolant-milling (Figure 4(b)), appeared to exhibit the
minimum number of stress induced cracks. On the
other hand, the hybrid-lubri-coolant-milled surface
was noticed with a greater number and the wet-lubri-
coolant-milled surface was noticed with the greatest
number of stress induced cracks. The observations
match well with the results of Figure 3(a). Moreover,
the possible reason of the minimum number of cracks
in the case of cryo-lubri-coolant-milling, is the non-
corrosive atmosphere of LN2 which diminishes the for-
mation of thermal cracks and its low temperature
Davis and Singh
which strongly opposes the material deformation, and
thus, causes the smooth and effective machining.36
Moreover, the cutting forces get reduced as the feed
and radial force get decreased with the rise in machin-
ing speed. At the higher levels of cutting speed, the
generated high temperature between cutting tool and
workpiece also assists in an easy removal of excess
material via a softening effect.37 However, the other
two lubri-coolant-milling conditions (Figure 4(a) and
(c)) consisted a comparatively higher temperature
than cryo-lubri-coolant-milling, which would allow
more amount of regional (local) softening, resulting
into the thermally induced surface damage via cracking
and adherence.7 Similar findings were observed in
Figure 5(a) to (c) also where cryo-lubri-coolant-milled
surface was found to be superior to hybrid-lubri-
coolant-milled surface followed by wet-lubri-coolant-
milled surface. However, in this case, the milled surfa-
ces exhibited the maximum damage and number of
cracks compared to Figure 4(a) to (c). The plausible
reason lies in the high level of feed rate which acceler-
ates the thermally induced smearing.37,38
Figure 6(a) to (c) also exhibit the similar trend
which was observed in Figures 4(a) to (c) and 5(a)
Figure 7. Surface milled at 56.52 m/min cutting speed with cryo-treated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
9
to (c). However, in terms of the surface cracks and
milling quality, an increase in the depth of cut also
resulted into poor surface integrity, which appeared
to be better than that of surfaces milled at high feed
rate. In the case of the high levels of feed rate and
depth of cut, the end mill gets more advanced into the
workpiece which localises a greater number of chips
at the end mill rake face. This further reduces the
cutting action of the end mill, moreover, it accompa-
nies a rubbing action caused by the accumulated chips
on the surface being milled, resulting into a more
deterioration of the surface quality.
Therefore, in addition to the SCC, some deep rub-
bing, and scratching feed marks can be seen in
Figures 5(a) to (c) and 6(a) to (c). Hence, in the
above three cases, cryo-lubri-coolant-milling appears
to be the most effective cooling technique, which
could most efficiently drive away the chips accumu-
lated on the end mill cutting edges. Moreover, the
surfaces with the poor finish quality can be inter-
preted as the ones with the non-uniformly distributed
oxide layers because of the presence of cracks and
feed marks. Therefore, all such surfaces can be more
prone to corrosion due to the establishment of
10
electrochemical potential difference at all the dam-
aged sites.38 However, another study on the machin-
ing of Mg alloy observed an enhanced resistance to
corrosion as a result of cryo-lubri-coolant machin-
ing.39 Hence, in the present study also, the cryo-
lubri-coolant-milling is likely to improve the corro-
sion resistance of the milled surface, which, however,
seeks to be experimentally endorsed.
Examination of the surfaces milled with cryo-treated end
mill. According to Figure 7(a) to (c), the improve-
ments in the surface finish quality of the milled sur-
faces with cryo-treated end mill at high level of
cutting speed can be sequenced in increasing order
as, wet followed by cryo and hybrid-lubri-coolant-
milling, which is also evident in compliance with the
observations displayed in Figure 3(b).
As mentioned previously that the low temperature
atmosphere during the machining at specific high
levels of input control variables might not be conve-
nient for the satisfactory performance of a cryo-
treated cutting tool since it can substantially raise
the hardness of the already hardened cutting tool
Figure 8. Surface milled at 0.60 mm/rev feed rate with the cryo-treated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
Proc IMechE Part C: J Mechanical Engineering Science 0(0)
(as a result of deep cryogenic treatment) and may
result into the breakage of cutting tool.13,15,23
This might be the credible cause why the hybrid-
lubri-coolant-milled surface (Figure 7(c)) was noticed
with better surface integrity compared to the cryo-
lubri-coolant-milled surface (Figure 7(b)), since
cryo-lubri-coolant-milling exhibited the lowest tem-
perature. The cryo-treated end mill could perform
better in a relatively warm milling environment
(Figure 7(c)) since it must have experienced a relative-
ly lesser breakage (as a result of lesser brittleness and
hardness) compared to the lowest temperature milling
environment (Figure 7(b)). The reasons of achieving a
poor surface quality at high levels of feed rate and
depth of cut are same as discussed in the previous
segment 3.2.1.
However, at the high feed rate and depth of cut,
the cryo-treated end mill was found to induce more
deterioration on the milled surfaces (Figures 8(a) to
(c) and 9(a) to (c)) compared to the untreated end mill
(Figures 5(a) to (c) and 6(a) to (c)). The major reason
of the same is the damage of more brittle and hard-
ened cutting edges of the cryo-treated end mill under
Davis and Singh
Figure 9. Surface milled at 1.5 mm depth of cut with the cryo-treated end mill amid (a) wet, (b) cryo, and (c) hybrid-lubri-coolant-
milling.
the influence of the lower milling temperatures and
larger cutting forces at high feed rate and depth of
cut. Further, as shown in Figures 8(a) to (c) and 9(a)
to (c), the milling with damaged cutting edges resulted
into the more surface cracking and impaired integrity.
EDS analysis
A recent study has reported a considerable modifica-
tion of hybrid-lubri-coolant-milled surface of Mg
alloy AZ31B as a result of an oxide layer formation.18
Hence, the same triggered the present study also to
examine the milled surfaces exhibiting improved sur-
face integrity for any possible surface modification.
Based on the findings of segment 3.1 and 3.2, the
surface milled with untreated end mill and cryo-lubri-
coolant-milling at 56.52 m/min cutting speed and the
surface milled with cryo-treated end mill and hybrid-
lubri-coolant-milling at 56.52 m/min cutting speed,
were found to possess the improved surface integrity.
Therefore, in this relation, the energy dispersive spec-
trometry (EDS) analysis was performed on both the
surfaces of interest achieved with the untreated as well
11
as cryotreated end mill. In addition, for a better com-
parison, the EDS analyses of the same surfaces before
milling have also been displayed for comparing the
weight percentage difference in the oxide content
after milling. As a result of the dynamic recrystalliza-
tion (DRX) and low temperature machining condi-
tions, the grain size gets positively altered and
retained in fine state, further inducing a passivation
layer with the help of the accumulated oxides, and
thus, termed as oxide layer.24
Some of the accumulated oxides are visible in the
form of a white precipitation at some locations on the
milled surfaces, shown in Figures 4 to 9. The passiv-
ation action of the oxide layer can significantly retard
the corrosion of degradable materials, when exposed
to corrosive atmosphere, by allowing a slower elec-
tron transmission to react with the base material.40
The percentage oxide content could be observed
with the help of EDS elemental mapping presented
in Figure 11. Figure 10(a) and (b), with Figure 11
reported a considerable increase in the oxide content
from 7.15 to 31.49 wt% (rise of approximately
24.34 wt%) on the surface milled with the untreated
12 Proc IMechE Part C: J Mechanical Engineering Science 0(0)

Figure 10. EDS plot of the (a) unmilled surface exhibiting 7.15 wt % oxide content, (b) surface milled with the untreated end mill and
cryo-lubri-coolant-milling at 56.52 m/min cutting speed, exhibiting 31.49 wt % oxide content, (c) unmilled surface, exhibiting 8.08 wt %
oxide content, and (d) surface milled with the cryo-treated end mill and hybrid-lubri-coolant-milling at 56.52 m/min cutting speed,
exhibiting 26.87 wt % oxide content.

end mill and cryo-lubri-coolant-milling. On the other
hand, Figure 10(c) and (d), with Figure 11 reported a
significant rise in the oxide content from 8.08 to
26.87 wt% (rise of approximately 18.79 wt%) on the
surface milled with cryo-treated end mill and hybrid-
lubri-coolant-milling. Therefore, it is evident that the
later surface possesses around 22.81% less oxide con-
tent compared to the former surface. The possible
reason of the former surface carrying a greater
number of oxides lies in having smaller grains,
which are capable of enhancing the electrochemical
reaction through the always moving electrons at the
Davis and Singh 13

Figure 11. EDS elemental mapping exhibiting (a) 31.49 wt % oxide content on the surface milled with the untreated end mill and
cryo-lubri-coolant-milling at 56.52 m/min cutting speed and (b) 26.87 wt % oxide content on the surface milled with the cryo-treated
end mill and hybrid-lubri-coolant-milling at 56.52 m/min cutting speed.

Figure 12. FESEM image displaying the passivation layer formed on (a) the surface (750  magnification) milled with the untreated
end mill and cryo-lubri-coolant-milling and (b) the surface (500  magnification) milled with the cryo-treated end mill and hybrid-lubri-
coolant-milling.
14
edges.41 Moreover, in Figure 10(d) the presence of
carbon (forming carbide) in higher content compared
to that of Figure 10(b), is also visible which is the
indicator of a substantial rise in the microhardness.
Additionally, some worn-out and migrated elements
from the end mill cutting edge such as Ti and W, are
also evident on the milled surfaces (shown in both
Figure 10(b) and (d)).
Assessment of the formed passivation (oxide) layer
thickness
This segment includes a further assessment of the pas-
sivation layer thickness formed over the selected
Figure 13. XRD plot of the the surface milled with the cryo-
treated end mill and hybrid-lubri-coolant-milling.
Figure 14. FESEM images of the worn-out faces of the cryo-treated end mills after using in the (a) cryo-lubri-coolant-milling and (b)
hybrid-lubri-coolant-milling at 56.52 m/min cutting speed.
Proc IMechE Part C: J Mechanical Engineering Science 0(0)
milled surfaces. Figure 12(a) and (b) demonstrate
the two milled surfaces with passivation layers of dif-
ferent thicknesses. A review reported that the cryo-
treated cutting tools could achieve oxide layer of uni-
form and lesser thickness compared to the ones
achieved via untreated cutting tools.8 Cryo-lubri-
coolant machining condition is known for achieving
the finest grain size on the machined surface.15
Consequently, the thickness of the finally formed pas-
sivation layer will be considerably affected. However,
SCC also plays an essential role in ascertaining the
thickness of the passivation layer. The surfaces prone
to SCC are susceptible to non-uniform distribution of
the passivation. Therefore, a significant variation
could be noticed in the oxide layer thickness on the
two milled surfaces. The surface milled with the
untreated end mill during cryo-lubri-coolant-milling
was found with a greater number of accumulated
oxides and thus, a non-uniformly distributed thick
oxide layer (19.23 mm), while the other surface
milled with the cryo-treated end mill during hybrid-
lubri-coolant-milling was found with lesser oxide con-
tent, and thus, a uniformly distributed thin oxide
layer (12.16 mm). These findings lie in accordance
with an already published article where the cryo-
treated end mill achieved a thinner and more uni-
formly distributed oxide layer compared to the
untreated end mill.18
Davis and Singh
X-ray diffraction examination of the milled surface
displaying the best improved surface integrity
Rigaku-TTRAX-III-XRD was used to execute the X-
ray diffraction examination of the surface milled with
the cryo-treated end mill amid hybrid-lubri-coolant-
milling. The reason of choosing only this surface for
the present analysis was its most improved surface
integrity, as reported by the previous sections.
CuKa radiation (k ¼ 1.5406 Å) was used for determin-
ing the phases and ascertaining the elements pos-
sessed by the passivation layer present on the
hybrid-lubri-coolant-milled surface. 0.01 step size
was used for collecting the required spectra. At a
speed of 2 /min, the continuous scanning was per-
formed in the 2h range of 20 to 95 .
Figure 13 demonstrates the XRD spectrum where
a-Mg is primarily present. Moreover, the existence of
b-phase (Mg17Al12) alloy was also spotted by the
XRD with some low intensity peaks such as 33 ,
42 , and 84 . a-Mg and ZnO could be indexed togeth-
er since no broadening behaviour was noticed.
Moreover, a-Mg and ZnO both exhibit hexagonal
crystalline structures and similar lattice constants.
The detection of ZnO with longer peaks confirm it
as the main oxide carrier present in the oxide (passiv-
ation) layer on the milled surface. The presence of
ZnO points toward the improved functional perfor-
mance to heal the accidental tissues and enhanced
corrosion resistance and biocompatibility of the
milled surface.42 Moreover, the combined effect of
oxides with b-Mg17Al12 can also substantially delay
the fast degradation of the surface.43 Hence, in addi-
tion to the EDS results, the XRD examination also
confirms a significant modification of the surface of
interest.
Morphology of the cryo-treated end mill
The damage at the cutting edge of the cryo-treated
end mill is evident in the case of cryo (Figure 14(a)) as
well as hybrid-lubri-coolant-milling condition (Figure
14(b)) at 56.52 m/min cutting speed. According to
Figures 3(b) and (d) and 11(b), the cryo-treated end
mill performed well and achieved improved surface
finish and microhardness during hybrid-lubri-cool-
ant-milling.
According to the discussion made in segment 3.1
and 3.2, the plausible reason of more wear of the
cryo-treated end mill compared to the untreated one-
during cryo-lubri-coolant-milling, is the additional
rise in its already increased brittleness as a result of
lowest temperature milling atmosphere. However, the
credible reason of the improved wear of cryo-treated
end mill in Figure 14(b) (in comparison to Figure 14
(a)) might be the favourable impact of temperature
and lubrication induced by hybrid-lubri-coolant-
milling on the refined and crystallographically aligned
a-phase particles and the reduced cobalt binder
15
b-phase. The reduced binding assists cryogenic treat-
ment in improving the thermal conductivity by
enlarging the dimensions of carbide particles.
Consequently, the cutting tools achieve better dissem-
ination of the generated heat at the cutting edge,
resulting into lesser damage and distortion (due to
the melting and wear) compared to the untreated
ones.8
Conclusions and future scope
The present research used a set of Ti-NAMITE
coated end mills in untreated and cryo-treated condi-
tions and achieved noteworthy findings during the
different lubri-coolant-milling operations of biocom-
patible Mg alloy AZ91D. However, some more latest
studies suggest the application of cutting tool textur-
ing with composite lyophilic/lyophobic wettabilities
and biocompatible hydrophilic coating for the bio-
medical applications.44,45 Moreover, the inclusion of
minimum quantity lubrication (MQL) is expected to
have a great significance as an effective lubri-coolant
in the extended study of this research.46
Based on the results obtained in this research, the
conclusions derived are summarized as follows:
• The untreated end mill functioned well in conjunc-
tion with the cryo-lubri-coolant-milling, which
consisted of the lowest temperature milling atmo-
sphere, and thus, could most effectively eliminate
the heat from the milling zone and induce an
enhanced surface integrity to the milled Mg alloy
AZ91D at high cutting speed.
• During the high cutting speed cryo-lubri-coolant-
milling, the untreated end mill attained 20.89%
and 31.42% lower surface roughness, and
11.89% and 20.13% higher microhardness than
that of hybrid and wet-lubri-coolant-milling,
respectively. However, in comparison to low cut-
ting speed, the untreated end mill achieved 29.82%
lower surface roughness and 14.63% higher micro-
hardness in the high speed cryo-lubri-coolant-
milling.
• The cryo-treated end mill performed best in asso-
ciation with hybrid-lubri-coolant-milling and
achieved the most improved surface integrity on
the milled Mg alloy AZ91D. Cryogenic treatment
capacitated the end mill with augmented mechan-
ical, thermal and metallurgical properties, which
considerably reduced the cutting and thrust forces.
• Amid the high cutting speed hybrid-lubri-coolant-
milling, the cryo-treated end mill attained 35.71%
and 48.07% lower surface roughness, and 13.58%
and 18.40% higher microhardness than that of
cryo and wet-lubri-coolant-milling, respectively.
However, in comparison to the low cutting speed,
the cryo-treated end mill achieved 46.12% lower
surface roughness and 15.73% higher surface
16
microhardness in the high cutting speed hybrid-
lubri-coolant-milling.
• In the present work, the improved surface integrity
of Mg alloy AZ91D suggests a substantial delay in
its biodegradation, when subjected to the corrosive
body fluid. However, the same needs to be validat-
ed via corrosion resistance testing as one of the
future scopes of the present work.
• The surfaces machined with both untreated and
cryo-treated end mill were noticed with passivation
(oxide) layers of significant thickness values, which
may be interpreted as a considerable surface mod-
ification. Nevertheless, the biocompatibility testing
of the modified surfaces will ascertain their bio-
medical applications.
Declaration of Conflicting Interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of
this article.
Funding
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
ORCID iD
Rahul Davis https://orcid.org/0000-0003-4795-9174
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