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Tailoring Surface Integrity of Biomedical Mg Alloy AZ31B Using Distinct End

Mill Treatment Conditions and Machining Environments

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DOI: 10.1007/s11665-020-05203-z

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Tailoring Surface Integrity of Biomedical
Mg Alloy AZ31B Using Distinct End Mill
Treatment Conditions and Machining
Environments

Rahul Davis & Abhishek Singh

Journal of Materials Engineering and

Performance

ISSN 1059-9495

J. of Materi Eng and Perform

DOI 10.1007/s11665-020-05203-z

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Tailoring Surface Integrity of Biomedical Mg Alloy AZ31B

Using Distinct End Mill Treatment Conditions
and Machining Environments
Rahul Davis and Abhishek Singh

Submitted: 15 June 2020 / Revised: 15 August 2020 / Accepted: 24 September 2020

Magnesium alloys are identified as the new generation degradable biomaterials in the biomedical industry.
They can prevent secondary operation for the removal of the inserted implant. Nowadays, sustainable
manufacturing is promoting the use of low-temperature machining environments over the traditional
means. Surface integrity characteristics of the machined surface and tool wear have always been some of
the key interests of the researchers. In this research, aluminum titanium nitride-coated cemented carbide
end mills were employed in an untreated and cryo-treated condition to machine the biomedical magnesium
alloy AZ31B. The experiments were designed using one-factor-at-a-time (OFAT) approach, and milling
operations were conducted under three different machining environments, namely wet, cryogenic, and
hybrid. Spindle speed, feed rate, and depth of cut were chosen as the input control variables for a com-
parative study to achieve lowest surface roughness and highest surface microhardness. The results dis-
played an improvement in the outcome at higher spindle speed (2800 rpm) and lower feed rate (80 mm/rev)
and depth of cut (0.5 mm) produced by untreated end mill during cryo-milling. However, the treated end
mill performed best with hybrid machining environment (simultaneous application of LN2 and cutting
fluid) during milling. Moreover, in this case, the accumulated oxides were found to form the most uniform
and thinnest passivation layer over the milled surface. Higher spindle speed in cryo-milling achieved 27.45
and 19.56% better surface finish than wet and hybrid-milling, respectively. Moreover, higher spindle speed
in cryo-milling achieved 14.46 and 8.72% higher surface microhardness than wet and hybrid-milling,
respectively. Higher spindle speed in hybrid-milling achieved 14.89 and 6.97% better surface finish than
wet and cryo-milling, respectively. Furthermore, higher spindle speed in cryo-milling achieved 7.69 and
4.10% higher surface microhardness than wet and cryo-milling, respectively.

biomedical devices are supposed to be removed (generally after

Keywords end mill wear, magnesium alloy AZ31B,
microhardness, surface cracks, surface roughness,
untreated and cryo-treated end mill, wet, cryogenic,
and hybrid-milling
1. Introduction
Annual medical data around the world record millions of
cases of bone fracture and damaged tissues because of
physical sicknesses and accidents. Many such fractures and
damages require placing and fixation of internal biomedical
devices (also known as biomedical implants) such as bone
plates, rods, screws, and nails for complete healing. However, a
large amount of stiffness of permanent metallic biomedical
implants often acts as a cause of stress shielding (referring
to reduction in bone density) of the damaged tissues or
fractured bones (Ref 1). This generally happens when the
YoungÕs modulus of metal alloys is much higher (100 to 200
GPa) than that of adjacent tissue or bone (10 to 45 GPa) to be
healed (Ref 2). In many cases, the implanted metal alloy
Rahul Davis and Abhishek Singh, Department of Mechanical
Engineering, National Institute of Technology Patna, Patna 800005,
India. Contact e-mails: rahul.me18@nitp.ac.in and abhishek.singh@
nitp.ac.in.
1 or 2 years) by a secondary surgery. The rising complications,
risks, and cost of this secondary surgery have led the
researchers to find some degradable biomedical devices as the
possible alternatives to overcome the existing challenges. Some
synthetic biodegradable polymers such as polylactide (PLA)
and polydioxanone (PDA) served the purpose in last decades
(Ref 1, 3), but their inappropriate and unsatisfactory perfor-
mance as bone implant has further pushed the researchers to
find some metallic degradable biomedical devices, among
which magnesium and its alloys are extremely popular
nowadays.
As stated by Liu et al. (Ref 4), bifunctional trace metallic
elements such as Ag, Ca, Sr, and Cu, when alloyed with Mg,
promote bone cell activation and also quicken the bone
formation. Mg alloys carry a density of 1.75-18.5 g/cm2, which
is remarkably close to the density of the human bone (1.8-2.1 g/
cm2). Magnesium and its alloys are biocompatible, osteocon-
ductive, lightweight, and load bearing biomaterials. In compar-
ison with different metal implants, the YoungÕs modulus of Mg
alloys is very identical to human cortical bone (Mg: 40-45 GPa,
Cortical bone: 10-27 GPa) unlike Ti-based alloys and 316L
stainless steel whose YoungÕs Modulus is 110 and 193 GPa,
respectively (Ref 5). An experimental study conducted by Wang
et al. (Ref 6) discussed the degradable property of magnesium
biomedical implants in the presence of human body fluid, which
further eliminates the requirement of another surgery for removal
of the implanted biomedical device. However, its degradation

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before complete healing or repair of the fractured bone (or
damaged tissue) appears as one of the greatest challenges faced
by the applications of magnesium alloy implants. To overcome
these challenges, several techniques have been developed and
proposed by various researches which can bring the degradation
rate of magnesium alloys in proportion to the healing rate of bone
or tissue. Uddin et al. (Ref 7) presented metal alloying techniques
(with Al, Zn etc.), coating techniques with corrosion resistant
layer (such as hydroxyapatite and calcium phosphate), and
mechanical techniques (such as burnishing, shot peening, and
machining), as the major methods used for that purpose.
Moreover, Uddin et al. (Ref 2) concluded that out of all the
mentioned techniques, improvement of surface integrity via
machining is not only an economic, quick, and easy method, but
also a means of revamping the fatigue strength of a biomedical
device. However, the type of machining operation, cutting tool,
machining environment, and achieved dimensional accuracies
noticeably affect the surface, mechanical, fatigue, and metallur-
gical characteristics of the mechanically finished part (Ref 8, 9).
In CNC machining operations, the presence of variable
speed, depth of cut, feed rate, cutting pressure, frictional force,
and excessive heat may cause softening, melting, and wear of
the cutting tool. Therefore, the cutting tool needs to exhibit
sufficient toughness, chemical stability, and electrical and
thermal conductivity (Ref 10, 11). Heat treatment, surface
coating, and cryogenic treatment are some popular modern
means for improving cutting tool performance by altering their
various properties significantly (Ref 12, 13). According to
several investigations, cryogenic treatment of cutting tools
improves their wear, mechanical, chemical, metallurgical,
thermal, and electrical properties noticeably. Subsequently,
the cryo-treated surface of cutting tool achieves a uniform
distribution of carbides (Ref 13-16).
Several investigations performed over the comparison
between untreated and cryo-treated cutting tools during CNC
machining, revealed the superiority of the later over the former
in terms of improved flank wear, hardness, fatigue resistance,
toughness, and thermal conductivity (Ref 16, 17).
Dhar and Kamruzzaman (Ref 14) reported a considerable
improvement in the life of cryo-treated tool by 38.6% in wet
machining, which was more in comparison to the dry machin-
ing. A few studies reported the application of wet (flood
cooling with the assistance of liquid coolant) and MQL
(minimum quantity lubrication) machining or cutting environ-
ments for obtaining the aimed results (Ref 17, 18). Nowadays,
literature also record a frequent use of liquid nitrogen as the
coolant in the cutting zone of CNC machining (also known as
cryogenic machining) to overcome the challenges faced by wet
and MQL techniques (Ref 19). This type of machining has been
proven to be an efficient environment-friendly mean of
achieving improved outcomes in terms of the desired degree
of dimensional accuracy, surface characteristics, fatigue life,
tool life, etc. It is due to the greater cooling efficiency of
cryogenic coolants, which could noticeably reduce the gener-
ated heat in the cutting zone (Ref 20). In an experimental
investigation, Scoop et al. (Ref 21) noticed that hybrid cooling
(cryogenic and MQL) could yield minimum cutting forces in
comparison with flood and cryogenic machining environments.
Al-Ghamdi et al. (Ref 22) compared the machinability of AISI
4340 and Ti-6Al-4V under CO2 snow-based cryogenic and
hybrid (CO2 snow + MQL) machining environments. The
hybrid machining could substantially reduce the cutting forces.
A limited literature on CNC end milling of biomaterials for
achieving improved surface integrity, is available. Moreover, a
comparative study among wet, cryogenic, and hybrid (wet +
cryogenic) machining environments using untreated and cryo-
treated (cryo-treated) end mills has not been reported until now.
This further suggests that opportunities are still available to
propose a more effective milling setup to enhance the process
performance and outcomes specifically for the manufacturing
of biomedical devices. Therefore, to bridge this gap, the present
research deals with the milling of biomedical Mg alloy AZ31B
with the aid of untreated and cryo-treated coated carbide end
mill in wet, cryogenic, and hybrid machining environments.
2. Experimental Procedure
The experimental procedure was as follows:
2.1 Design of Experiment via One-Factor-at-a-Time (OFAT)
Approach
In the present work, the experiments were designed using
one-factor-at-a-time (OFAT) approach, which is basically one
of the statistical approaches of design of experiment (DOE).
This approach allows only one factor (input control variable) to
vary at a time, keeping rest of the experimental input control
variables as constant. This is how it can reveal and interpret the
actual influence of each input control variable on the process
more specifically. The experimental runs are repeated for each
input control variable. However, it does not include the study
of interactions among these variables (Ref 23).
2.2 Experimental Details
2.2.1 Workpiece Specifications. The work material used
for the experiments was commercially available magnesium
alloy AZ31B, which is one of the most widespread alloys of
magnesium used in producing the degradable biomedical
implants. It possesses high strength suitable for biomedical
applications. Hence, to machine this biomaterial, the smooth-
ness of the surface is a necessity regarding acclamatory residual
stress which is a form of subsurface properties. Table 1 displays
the weight percentage of the constituents present in it. The
composition of the workpiece material was measured (via
positive material identification (PMI) technique) and provided
by the supplier (Petromet Flange Inc., Mumbai, India). The
Table 1 Percentage contribution of elements present in
magnesium alloy AZ31B
Element Weight percentage
Aluminum 3.20
Zinc 1.30
Silicon 0.10
Manganese 0.18
Calcium 0.03
Copper 0.04
Magnesium 96.7
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Table 2 Specifications of milling setup for the proposed machining runs
Specifications Units
CNC
Software
Main power supply
Spindle motor capacity HP
Programmable spindle speed rpm
Feed rate mm/rev
Depth of cut mm
End mill
End mill length mm
End mill diameter mm
Coating
Hardness HV
Thermal stability C
Machining environment during milling
Coolant
Cryogenic medium (LN2)
Liquid nitrogen container (Cryocan)
Liquid nitrogen withdrawal device
Air compressor
specifications of the milling setup are shown in Table 2. This
table demonstrates the various features of the milling machine,
input control variables (spindle speed, feed rate, and depth of
cut), and machining environments used to execute the proposed
milling operations. The specifications of the end mill tool have
also been displayed.
2.2.2 Milling Setup Specifications. As discussed by
Fang et al. (Ref 24), flame ignition and flank built-up are
some of the problems when machining magnesium alloys,
which lead to poor surface quality of the machined biomaterial
as a result of the production of erratic machining forces.
Optimal input control variables must be adopted to get
favorable results from the machining of these materials. In this
relation, Abhijith et al. (Ref 25) examined the changes on
biodegradable AZ31 magnesium alloy surface in response to
optimal variation in depth of cut, feed rate, and cutting speed
during dry face milling. Bosse et al. (Ref 26) experimentally
investigated the milling of magnesium alloys with lower values
of feed rate and higher values of cutting speed. Both the
investigations could substantially improve the machinability,
surface integrity, and degradation rate. Figure 1 is the repre-
sentation of experimental plan and Fig. 2 of the milling setup,
showing the cooling medium dispensation arrangements, CNC
XL Mill, and liquid nitrogen tank and its accessories.
2.2.3 End Mill Treatment Condition. On the basis of
temperature range, Akincioğlu et al. (Ref 10) classified
cryogenic treatments as: (i) shallow (temperature ranging from
80 to 140 C) and (ii) deep (temperature ranging from
80 to 140 C). Moreover, Bensely et al. (Ref 27) pointed
out liquid nitrogen as the recommended cryogenic environment
by mostly researchers since it contributes around 78.03% of the
atmosphere. In addition, according to a comprehensive review,
soaking temperature was reported to be the most influential
factor on the wear resistance (Ref 10). This suggests that the
determination of correct soaking stage duration and temperature
Journal of Materials Engineering and Performance
XL Mill
PC based 3 axis continuous path control system
CAM software
230 V, single phase, 50 Hz
0.5
1400 2800
80 120
0.5 1.0
Kyocera 48509 solid carbide
4 Flute, SER 01S
40
6
Aluminum titanium nitride (Ti-NAMITE)
3700
1100
Wet Cryogenic Hybrid
Coolant LN2 Coolant + LN2
Zed-plus
Liquid nitrogen (at 196 C)
Cryogem PS 34
Flow rate—5 L/min
MEI YI—ZM-0.12/8
is crucial. Further, sudden exposition of the sample to cryo-
genic environment may develop micro-cracks on the sample
surface owing to thermal impact (Ref 28).
Some studies reported a common reduction of 5-6% in the
cutting tool flank wear in addition to a considerable improve-
ment in hardness, abrasive wear, nose wear, and pull-out and
segregation of carbide grains as a result of cryogenic treatment
(Ref 29, 30). Cryogenic treatment of solid carbide (WC)
primarily leads to the formation of stabilized and finer g-phase
particles. Moreover, size of a-phase and density of b-phase are
increased. These altered features can further lead to enhanced
resistance of cobalt binder toward corrosion. In addition,
enlarged adjacent grain structures of the material may lead to a
considerable rise in thermal conductivity of the solid carbide
(WC). However, in the case of consistently spread and properly
refined g-phase particles, wear resistance and toughness are
expected to be significantly improved. Although, in the
presence of hard g-phase particles, a substantial increase in
the brittleness of the material could be noticed, which may
further cause early tool failure (Ref 29). The other study
experimentally investigated the properties of untreated and
cryo-treaded solid carbide cutting tools using magnetic satura-
tion and coercivity tests. The results revealed that no alteration
was observed in the amount of carbon present, which ascertains
that no precipitation of eta-carbides (g-carbides) could occur.
However, FCC to HCP phase transformation of cobalt took
place, which is mainly responsible for improving the perfor-
mance of carbide cutting tools (Ref 30).
The present research used liquid nitrogen assisted deep
cryogenic treatment with a soaking time period and temperature
of 24 h (rate of cooling of 1 C/min) and 196 C,
respectively, to enhance the performance of a set of solid
carbide end mills. Figure 3 shows the deep cryogenic treatment
cycle.
 Author's personal copy

Fig. 1 Experimental plan for milling process

2.2.4 Machining Environment Specifications. In the

present work, dry milling of Mg alloy AZ31B was not
employed since this alloy of magnesium is also a highly
flammable material (Ref 24). Moreover, it was revealed that dry
milled surfaces carry a greater number of defects than wet and
cryo-milled surfaces (Ref 8). Therefore, the present work
consists of several milling experimental runs with the applica-
tion of an untreated and cryo-treated end mill under three
different machining environments: wet, cryogenic, and hybrid.
Figure 4 is the demonstration of the schematic diagrams of the
three machining environments during milling. Wet machining
environment (Fig. 4a) consisted of the use of liquid coolant,
cryogenic machining environment (Fig. 4b) used liquid nitro-
gen (LN2), and hybrid machining environment (Fig. 4c)
consisted of the application of both liquid coolant and LN2
simultaneously. A set of an untreated and a cryo-treated coated
aluminum titanium nitride end mills was employed for the
milling operations.
2.2.5 Output Machining Characteristics. As outlined
by Jawahir et al. (Ref 31) and Kaynak et al. (Ref 32),
machining-induced surface integrity characteristics such as
phase transformation, surface roughness, residual stress, surface
microhardness, corrosion resistance, residual stress, and surface
topography, have attracted the attention of mostly researchers.
The two-leading machining-induced surface integrity charac-
Fig. 2 Experimental setup for milling process teristics chosen for the current research were surface roughness
(lm) and microhardness (HV).
A degradable implant surface with a considerable number of
defects is more prone to corrosion and thus early degradation.
The defects on the mechanically processed surfaces can behave
as local crack initiators when subjected to any type of loading.
Bruschi et al. (Ref 33) reported that corrosion resistance of the
machined surfaces largely depends on the produced surface
finish. Therefore, surface with the lowest roughness can be
considered as one with highest corrosion resistance. According
to Huja et al. (Ref 34), the approximation of mechanical
characteristics enveloping an implanted device, can be per-
formed with the help of surface microhardness. The surface
properties of the host bone tissue such as microhardness, play a
vital role in ascertaining the stability of a biomedical implant.
Moreover, this microhardness can also describe the trend of the
Fig. 3 Deep cryogenic treatment cycle
host tissue maturation and its mechanic resistance (Ref 35).
Therefore, the proper regulation of these two surface integrity

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Fig. 4 Schematic diagrams of (a) wet, (b) cryogenic, and (c) hybrid machining environment

Table 3 Milling operations under the three cooling environments using untreated end mill
Wet-milling Cryo-milling Hybrid-milling

Spindle speed (rpm) T-I T-II T-III Mean T-I T-II T-III Mean T-I T-II T-III Mean

1400 Surface roughness (lm)

0.54 0.65 0.64 0.61 0.47 0.57 0.47 0.51 0.55 0.65 0.51 0.57
Micro hardness (HV)
87.6 79.7 86.2 84.5 87.3 95.1 92.7 91.7 86.8 83.4 91.7 87.3
2800 Surface roughness (lm)
0.51 0.49 0.53 0.51 0.37 0.36 0.38 0.37 0.47 0.49 0.42 0.46
Micro hardness (HV)
88.3 91.8 81.2 87.1 102.7 97.6 98.8 99.7 91.7 97.7 93.2 94.2
Constant input control variable: feed rate and depth of cut
Feed rate (mm/rev) Surface roughness (lm)
80 0.78 0.74 0.73 0.75 0.65 0.64 0.69 0.66 0.69 0.71 0.73 0.71
Micro hardness (HV)
82.7 79.4 80.4 80.9 81.3 81.9 85.2 82.8 81.1 79.8 83.3 81.4
120 Surface roughness (lm)
0.98 0.97 1.02 0.99 0.80 0.79 0.84 0.81 0.86 0.88 0.93 0.89
Micro hardness (HV)
76.3 74.6 73.8 74.9 81.4 77.3 76.9 79.2 74.9 78.4 75.9 76.4
Constant input control variable: spindle speed and depth of cut
Depth of cut (mm) Surface roughness (lm)
0.5 0.74 0.73 0.78 0.75 0.57 0.59 0.61 0.59 0.64 0.65 0.69 0.66
Micro hardness (HV)
80.3 78.2 82.7 80.4 79.9 85.1 81.6 82.2 83.9 79.8 80.9 81.5
Surface roughness (lm)
1.0 0.85 0.87 0.83 0.85 0.69 0.71 0.70 0.70 0.79 0.77 0.81 0.79
Micro hardness (HV)
78.9 76.2 75.3 76.8 81.7 78.9 82.1 80.9 81.2 77.9 79.7 79.6

Constant input control variable: spindle speed and feed rate

characteristics can substantially restrict the defects in manu-
factured surfaces and thus, enhance the corrosion resistance
(Ref 36).
A surface roughness tester (Make/Model: Precise/TR110
Plus) was used to measure the surface roughness values. The
measuring technique involved sliding the pointer of the tester
with a sampling length of 1 mm on the surface of the machined
workpiece. For measuring microhardness, the diamond indenter
of a Vickers hardness tester (Make/Model: Blue Star Ltd./
BSHT-FHV1-50) was pressed into the machined area (with a

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Table 4 Milling operations under the three cooling environments using cryo-treated end mill
Wet-milling Cryo-milling Hybrid-milling

Spindle speed (rpm) T-I T-II T-III Mean T-I T-II T-III Mean T-I T-II T-III Mean

Surface roughness (lm)

1400 0.61 0.59 0.57 0.59 0.53 0.55 0.60 0.56 0.54 0.50 0.51 0.52
Micro hardness (HV)
84.9 85.3 85.4 85.2 86.4 86.1 86.1 86.2 89.2 89.5 89.4 89.3
Surface roughness (lm)
2800 0.48 0.45 0.48 0.47 0.42 0.41 0.45 0.43 0.40 0.37 0.43 0.40
Micro hardness (HV)
87.2 86.7 87.4 87.1 90.5 89.8 90.1 90.1 94.2 93.6 93.7 93.8
Constant input control variable: feed rate and depth of cut
Feed rate (mm/rev) Surface roughness (lm)
80 0.71 0.69 0.72 0.71 0.74 0.76 0.75 0.75 0.64 0.69 0.68 0.67
Micro hardness (HV)
79.9 80.4 80.2 80.2 79.7 79.8 79.9 79.8 81.5 81.5 81.8 81.6
120 Surface roughness (lm)
0.82 0.85 0.86 0.84 0.97 0.91 0.94 0.94 0.78 0.81 0.81 0.80
Micro hardness (HV)
75.6 75.7 76.3 75.9 68.3 68.7 68.5 68.5 77.8 78.5 78.3 78.2
Constant input control variable: spindle speed and depth of cut
Depth of cut (mm) Surface roughness (lm)
0.5 0.69 0.65 0.67 0.67 0.66 0.69 0.71 0.69 0.57 0.58 0.61 0.59
Micro hardness (HV)
82.9 82.4 82.3 82.5 81.4 81.3 81.4 81.4 83.3 83.7 83.2 83.4
Surface roughness (lm)
1.0 0.73 0.69 0.70 0.71 0.76 0.78 0.79 0.77 0.59 0.60 0.61 0.60
Micro hardness (HV)
78.3 78.3 78.0 78.2 71.8 71.6 72.2 71.9 79.7 79.8 79.9 79.8
Constant input control variable: spindle speed and feed rate

load of 100 gf for approximately 10 s), which left a right
pyramid shaped impression. Later, the impression size was
measured using the diagonal lengths for finally calculating the
microhardness value. Generally, similar test conditions restrict
the microhardness values within a limited spectrum. The
processes of measuring surface roughness and microhardness
were repeated at three different places on a machined region (of
each specimen) followed by averaging all the three values for
each machined specimen.
3. Analysis and Discussion
3.1 Results Obtained from Experimental Trial Runs
As discussed above, this study performed a series of
experimental runs based on one-factor-at-a-time approach. The
input control variables tried by OFAT approach for the present
research, are tabulated in Tables 3 and 4. The obtained
responses are also presented in the same. Table 3 displays the
results observed in milling operations performed by untreated
end mill, while Table 4 displays the observations achieved by
cryo-treated end mill. According to Table 3, the lowest surface
roughness and highest microhardness values were achieved by
the untreated end mill at higher spindle speed (2800 rpm)
during cryo-milling, followed by hybrid and wet-milling. As
displayed by Table 4, the lowest surface roughness and highest
microhardness values were achieved by the cryo-treated end
mill at higher spindle speed during hybrid-milling, followed by
cryogenic and wet-milling. With a rise in the feed rate, some
places on the workpiece surface were left uncut and thus, the
same increased the surface roughness. Hence, lower the feed
rate better the surface roughness. However, with increase in
spindle speed, surface roughness decreased. It happened
because higher speeds reduce the cutting forces. Moreover,
better surface finish is obtained due to less built-up edges (Ref
12). Therefore, in Tables 3 and 4, increasing feed rate and
depth of cut values adversely affected the surface roughness
and microhardness values in all the machining environments.
3.2 Comparative Analysis of Surface Roughness Produced
by Untreated and Cryo-treated End Mill
Figure 5 presents plots comparing the effects of untreated
and cryo-treated end mill, varying input control variables, and
different machining environments on the roughness of the
milled surface. From Fig. 5(a), the significant effect of
untreated end mill at higher spindle speed (2800 rpm) on the
surface roughness amid cryo-milling, is evident. However,
Fig. 5(b) and (c) demonstrate a considerable rise in the
roughness with the increase in feed rate and depth of cut.
These findings fall in strong compliance with the previously
achieved results where higher feed rate and depth of cut
assisted in increasing the power consumption and cutting force,
which further resulted in higher surface roughness (Ref 12, 37).
However, cryo-milling achieves lowest surface roughness in
each case with untreated end mill. The possible reason of this

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Fig. 5 Plots comparing the effects of untreated and cryo-treated end mill, varying input control variables, and different machining environments
on surface roughness
reduced roughness might be the diminished smearing and
plucking mechanism caused by cryo-milling (Ref 38). Cryo-
treated end mills must have exhibited improved thermal
conductivity because of carbide particles with bigger size and
refined grains, which aid in enhanced heat dissipation (Ref 12,
30). The same must be the credible reason of the improvement
in surface roughness in the case of wet-milling at a higher
spindle speed by cryo-treated end mill compared to the
untreated end mill. This finding goes well with the results
reported by several authors, in which an improved surface
finish was obtained via cryo-treated cutting tools (Ref 39, 40).
However, cryogenic machining environment increases the
brittleness of the cutting tool. In addition, higher speeds can
Journal of Materials Engineering and Performance
develop micro-cracks on the tool surface. Higher feed rate and
depth of cut can promote wear on the brittle tool surface.
Moreover, cryogenic treatment considerably improves the
hardness of cutting tools (Ref 16, 31). Therefore, the cryo-
treated end mill must have experienced more hardness and
brittleness during cryogenic followed by hybrid machining
environments. However, this cryo-treated end mill might have
been susceptible to less wear but more tool failure (by tool
breakage) in cryogenic machining environment. This is the
possible reason why the surface roughness increased as the
temperature of machining environment went down from wet to
hybrid, and then from hybrid to cryogenic.
 Author's personal copy

Fig. 6 Plots comparing the effects of untreated and cryo-treated end mill, varying input control variables, and different machining environments
on surface microhardness

3.3 Comparative Analysis of Microhardness Produced and thermal softening (Ref 41). Moreover, the grain refinement
by Untreated and Cryo-treated End Mill into finer grains also increases the surface hardness signifi-
cantly. In addition, improved surface finish is the indicator of
Figure 6 presents plots comparing the effects of untreated
improved surface microhardness. These are the reasons why the
and cryo-treated end mill, varying input control variables, and
highest microhardness values were observed in the cryo-milled
different machining environments on the microhardness of the
surfaces followed by hybrid and wet-milled surfaces. Further,
milled surface. Figure 6(a) demonstrates the highest value of
as stated by Klocke et al. (Ref 42), the improved hardness is
surface microhardness at the higher spindle speed with the aid
considered as the indicator of improved wear and corrosion
of untreated end mill amid cryogenic milling. The plausible
resistance.
cause is the fact that liquid nitrogen rapidly cools the surface
As discussed in the previous Sect. 3.2, cryo-treated end mill
which hardens the material. According to the several scientific
is able to achieve enhanced surface finish only in the
studies, the microhardness values of the cryo-machined part
environment of wet-milling at higher spindle speed, owing to
(machined under the cryogenic cooling) are found to be
the excessive end mill wear in the machining environments
enhanced because such a low temperature causes strain
with lower temperatures. Therefore, the surfaces with poor
hardening on the surface and decreases the generated heat,

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Fig. 7 Milled surfaces produced by untreated end mill at 2800 rpm spindle speed during (a) wet, (b) cryogenic, and (c) hybrid machining
environment

finish also display lower microhardness. That is the reason the specimen experiencing thermal cracking, is generally smaller
plots in Fig. 6(b) and (c) display lower values of surface than the plastic deformation zone (Ref 44). Hence, thermal
microhardness. cracks can be induced on the machined surface but are
restricted to a limited volume. However, conventionally
3.4 Morphological Study of Milled Surfaces by Untreated machined Mg AZ31 primarily experiences stress-induced or
End Mill stress corrosion cracking (SCC) due to the imparted residual
stress or the joint impact of corrosive environment and tensile
This section includes the morphological studies of only
stress (Ref 45). According to a comprehensive review, this
those milled surfaces which achieved the highest degree of
thermal cracking can be avoided on the surface and subsurface
surface finish and lowest values of microhardness. Field-
of Mg AZ31B by reducing the temperature of the machining
emission scanning electron microscope (GeminiSEM 500,
environment. The review records several researchers adopting
Zeiss) was employed to examine the morphology and defects
cryogenic machining environment as an effective alternative to
(at a magnification of 15009) present in the surfaces milled
overcome thermal cracking (Ref 32). Moreover, Mg alloys
under different conditions. In conventional machining, these
exhibit a very weak resistance toward corrosion even in the
surface defects (also termed as ‘‘cracks’’) are basically caused
environment of water and dilute electrolyte solutions (Ref 46).
because of residual stress imparted by the variation in thermal
Several studies reported that magnesium alloys undergo stress
and mechanical effects. Thermal variations are originated by
corrosion cracking due to the presence of corrosion pits (due to
the friction occurring at the cutting tool–workpiece–chip
corrosive environment) at different sites on the surface and
interface and can be more dominant than mechanical effects
subsurface of the workpiece material. In addition, a consider-
in the presence of a considerable rise in feed rate (Ref 43, 44).
able rise in surface roughness and hardness can also contribute
In alignment to this fact, a study outlined that in addition to
toward the same (Ref 43, 47). Therefore, based on the available
stress-induced cracking amid conventional machining, Mg
literatures, in the present study also, Mg AZ31B samples were
AZ31 can also exhibit some thermal cracks when exposed to
susceptible to exhibit both stress-induced (or stress corrosion
sudden temperature changes, leading to thermal shock and
cracking) and thermal cracks depending on the effects of
stress. However, the volume of a conventionally machined
different machining environments and input control variables.

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Fig. 8 Milled surfaces produced by untreated end mill at 120 mm/rev feed rate during (a) wet, (b) cryogenic, and (c) hybrid machining
environment
On the basis of already published extensive research on the
machining of Mg AZ31B, the present study designates the
thinner cracks (over a relatively smaller volume) as thermal
cracks and the bigger and deeper cracks (over the bigger
volume) as the stress-induced or stress corrosion cracks.
Figure 7(a), (b), and (c) present the morphology of the
milled surfaces produced by untreated end mill at higher
spindle speed (2800 rpm) under wet, cryogenic, and hybrid
machining environments, respectively. Figure 7(a) exhibits
both thinner and wider types of cracks at various sites. Firstly,
as discussed above, the thinner and smaller sized cracks are
probably the thermal cracks due to the temperature variation in
the presence of cutting fluid. Secondly, the wider and deeper
cracks can probably be the stress-induced or corrosion cracks
since the environment of cutting fluid may act as corrosive
environment (Ref 45, 46). In Fig. 7(b), the milled surface
produced under cryogenic machining environment carried least
number of cracks. These cracks are probably stress-induced
cracks (purely induced by stress) since liquid nitrogen envi-
ronment is non-corrosive and eliminates thermal cracking to a
great extent, and therefore, the probability of stress corrosion
cracking is also less. Figure 7(b) is found to be in good
agreement with the lowest surface roughness at higher spindle
speed value obtained via cryo-milling. Villegas and Shaw (Ref
48) discovered that cryo-milling possessing the lowest temper-
ature, acts as a hindrance against material deformation during
cryo-milling. This further results into the most effective tearing
and thus, machining. However, according to another study, wet
and hybrid machining environments are expected to have more
local softening since they possess relatively higher machining
temperatures. This would further lead to thermally activated
smearing and favoring adhesion (Ref 8). In Fig. 7(c) both types
of cracks can be seen, since in the hybrid-milling the presence
of cutting fluid could promote corrosive environment and
thermal variations as well.
Figure 8(a), (b), and (c) display the influence of higher feed
rate (120 mm/rev) on the milled surfaces. The quality of the
surface (in terms of roughness and cracks) is evident on the wet
(Fig. 8a), cryo (Fig. 8b) and hybrid-milled (Fig. 8c) surfaces.
The wet-milled surface displays the roughest surface with the
greatest number of cracks, followed by hybrid cryo-milled
surfaces. In this case also, the reasons behind the formation of
different types of cracks lie in accordance with Fig. 7(a), (b),
and (c). However, in this case the probability of the formation
of number of thermal cracks is more due to higher feed rate,
which would promote the domination of thermal effects over
mechanical effects (Ref 44, 45).
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Fig. 9 Milled surfaces produced by untreated end mill at 1 mm depth of cut during (a) wet, (b) cryogenic, and (c) hybrid machining
environment

Figure 9(a), (b), and (c) demonstrate the impact of deeper 3.5 Morphological Study of Milled Surfaces by Cryo-treated
depth of cut (1 mm) on the milled surface. This impact of End Mill
deeper depth of cut is found to be almost similar to the
In accordance with Sect. 3.4, this section also has the similar
influence of feed rate, but with relatively lesser number of
grounds for the formation of different types of surface
cracks. However, in this case also, cryo-milled surface (Fig. 9b)
roughness and cracks under same machining environments.
is found to be superior to other two surfaces (Fig. 9a and c), in
Figure 10(a), (b), and (c) present the morphology of the milled
terms of surface roughness and cracks. Moreover, wet-milled
surfaces produced by cryo-treated end mill at higher spindle
surface was found with poorest surface roughness and greatest
speed (2800 rpm) under wet, cryogenic, and hybrid machining
number of cracks. Hybrid-milled surfaces fell somewhere in the
environments, respectively. Figure 10(a) exhibits roughest
middle of cryo and wet-milled surfaces, in terms of roughness
surface with both thinner and wider types of cracks at various
and cracks. Here again, the similar reasons (as discussed in
sites. In the case of Fig. 10(b), again a sound agreement is
Fig. 7a, b, and c) are responsible for the formation of different
found with the lowest surface roughness at higher spindle speed
types of cracks. Untreated end mill could produce least number
value obtained via cryo-milling. In the case of Fig. 10(c)
of defects under cryogenic cooling followed by hybrid and wet
(similar to Fig. 7c), both types of cracks are evident owing to
cooling environments. The greater number of defects observed
the fact of the presence of cutting fluid in the hybrid-milling,
in hybrid and wet-milled surfaces degrades the oxide layers
which could promote both corrosive environment and thermal
formed amid milling. This gives rise to the settlement of the
variations. Here, the milled surface (Fig. 10c) produced under
electrochemical potential difference in all the defective regions
hybrid machining environment, carried least number of cracks.
or locations, which may further expose all such regions to
As discussed in Sect. 3.2, low temperature of the machining
corrosion (Ref 49). Liu and Frankel (Ref 50) noticed that
environment adversely affects the performance of cryo-treated
cryogenic machining effectively imputed grain refinement on
cutting tool at higher feed rate and deeper depth of cut (Ref 19).
Mg alloy AZ31B toward the improvement of corrosion
Therefore, the cryo-treated end mill might have experienced
resistance. Therefore, cryo-milled surface might display higher
less hardening and brittleness, and thus, less wear, in hybrid-
corrosion resistance, which needs to be further validated.
milling than in cryo-milling. This might be the possible reason

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Fig. 10 Milled surfaces produced by cryo-treated end mill at 2800 rpm spindle speed during (a) wet, (b) cryogenic, and (c) hybrid machining
environment

why hybrid-milled surface exhibited best surface finish and oxide content present on the milled surface along with other
least number of cracks. As outlined in Sect. 3.2, higher feed rate elements. FESEM shows the most uniform distribution of the
(120 mm/rev) and deeper depth of cut (1 mm) are responsible accumulated oxides on the milled surface. Some Ti and W
for a poor surface finish. Therefore, cryo-milled surfaces contents are also visible in all the EDS figures, which shows the
(Fig. 11b and 12b) produced by cryo-treated end mill at higher worn-out end mill particles accumulated on the milled surface.
feed rate and deeper depth of cut, being subjected to the lowest
temperature, exhibit the greatest number of cracks followed by 3.6 X-ray Diffraction Analysis of Milled Surfaces
wet-milled surfaces (Fig. 11a and 12a). However, hybrid-milled
X-ray diffraction (XRD) of the milled surfaces of interest
surfaces (Fig. 11c and 12c) display the best surface in terms of
was performed by Rigaku-TTRAX-III-XRD to obtain the
minimum surface roughness and number of cracks.
crystalline spectra and confirm the detailed chemical compo-
Further, milled surfaces of interest were also analyzed by
sition of the surface. Crystalline phases were evaluated by x-ray
Energy-Dispersive Spectrometry (EDS-GeminiSEM 500,
diffraction using CuKa radiation (k = 1.5406 Å). Spectra were
Zeiss). Figure 13 depicts EDS and FESEM image of the
collected with a step size of 0.01, continuous scan with a speed
surface milled by untreated end mill amid cryo-milling at
of 2/min, and over the 2h range 20 to 95.
2800 rpm spindle speed. EDS and FESEM show the maximum
Figure 16 presents XRD plots demonstrating a comparison
amount of oxide content present on the milled surface along
among the three surfaces of interest of this study. The XRD
with other elements. Figure 14 shows EDS and FESEM image
spectrum shows mainly the presence of a-Mg. Meanwhile, the
of the surface milled by cryo-treated end mill amid cryo-milling
XRD detected the presence of phase b-phase (Mg17Al12) alloy
at 2800 rpm spindle speed. The damaged surface with cracks is
as shown by the low intensity peak at 31. ZnO phases could
clearly visible. FESEM shows the non-uniform distribution of
also be indexed along with Mg peaks and did not exhibit a
the accumulated oxides on the milled surface.
broadening behavior, as both present hexagonal crystalline
Figure 15 demonstrates EDS and FESEM image of the
structures and similar lattice constants. It is believed that ZnO
surface milled by cryo-treated end mill amid hybrid-milling at
presence is possibly due to oxide deposition from the
2800 rpm spindle speed. EDS shows the minimum amount of

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Fig. 11 Milled surfaces produced by cryo-treated end mill at 120 mm/rev feed rate during (a) wet, (b) cryogenic, and (c) hybrid machining
environment

machining process, as the intensity of peaks increases for cryo-
milled surface by untreated end mill, for example peaks at 36,
48, and 57. All the three surfaces contain accumulated oxides
in different measures. ZnO is an indicator of improved
corrosion resistance, antimicrobial, antibacterial, and biocom-
patible behavior of the machined surface (Ref 51). Moreover,
zinc ions tend to promote the cellular response which assists in
quick recovery of the damaged tissues. Also, the presence of b-
Mg17Al12 coupled with oxide significantly decelerates the
degradation of the implant surface. Evidence of b-Mg17Al12
phase at grain boundaries depicts the rise in Al content by more
than 1%. The same can facilitate the ease of machining (Ref
52). Therefore, the collective presence of these layers was
identified as the favorable modification of the milled surface.
However, the amounts of ZnO and b-Mg17Al12 are found to be
quite different on each milled surface. Surface milled by
untreated end mill during cryo-milling depicts the largest
amount of these elements (ZnO and b-Mg17Al12), which is an
indicator of the thickest layer formed by the accumulated
oxides (can be termed as ‘‘oxide layer’’). Surface milled by
cryo-treated end mill contains the least amount of these
elements in the case of hybrid-milling, followed by cryo-
milling. Therefore, XRD plots also convey this confirmation
that the layer of the accumulated oxides formed by cryo-treated
end mill during hybrid-milling, is found with the lowest
thickness among all the layers.
3.7 Morphological Study of the Accumulated Oxides
The accumulated oxides form a layer on the machined
surface which has the ability to delay the corrosion of a
degradable material in corrosive environment by reducing the
electron transfer for electrochemical reaction with the base
metal. This layer hinders the unnecessary migration of metal
ions from implant material to human body, and thus, shuns the

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Fig. 12 Milled surfaces produced by cryo-treated end mill at 1 mm depth of cut during (a) wet, (b) cryogenic, and (c) hybrid machining
environment

Fig. 13 EDS and FESEM image (at 50009 magnification) of the surface milled by untreated end mill amid cryo-milling at 2800 rpm spindle
speed, 0.5 mm depth of cut, and 80 mm/rev feed rate

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Fig. 14 EDS and FESEM image (at 50009 magnification) of the surface milled by cryo-treated end mill amid cryo-milling at 2800 rpm
spindle speed, 0.5 mm depth of cut, and 80 mm/rev feed rate

Fig. 15 EDS and FESEM image (at 50009 magnification) of the surface milled by cryo-treated end mill amid hybrid-milling at 2800 rpm
spindle speed, 0.5 mm depth of cut, and 80 mm/rev feed rate

occurrence of cytotoxicity and unwanted reactions (Ref 53). So,

Fig. 16 XRD plots of three milled surfaces by different end mills
under distinctive machining environments
its detailed study is an essential part of the present research. In
an experimental study, Park et al. (Ref 54) observed that
machining with cryo-treated cutting tool achieved more
uniform and thinner oxide layer. Therefore, this section has
been made a part of this current study to present a discussion
over the oxide layers formed during cryo and hybrid-milling by
cryo-treated end mill at higher spindle speed. At the shown
microstructure in Fig. 17(a) and (b), enlarging spreads of the
influenced layer facilitated by cryogenic cooling, are evident.
During the grain refinement process, the expected grain growth
caused by the high temperatures (in the machining zone) is
effectively controlled by cryogenic cooling (Ref 32). Dynamic
recrystallization (DRX) causes the formation and retaining of
refined grains, which further leads to such a featureless oxide
layer. Moreover, this oxide layer is recognized as a passivation
layer, and its formation is reported because of the formation of
more compressed surfaces amid low-temperature milling (Ref
55). As outlined by some studies on machining of AZ31B,
among different machining environments, only cryogenic

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Fig. 17 Accumulated oxides forming a passivation layer during (a) cryo-milling and (b) hybrid-milling by cryo-treated end mill at 2800 rpm
spindle speed
Fig. 18 FESEM image (at 10009 magnification) of the
accumulated oxides (forming a passivation layer) during hybrid-
milling by cryo-treated end mill at 2800 rpm spindle speed
machining environment could generate compressive residual
stress both axially and circumferentially. Moreover, compres-
sive residual stresses present inside the work material reduce
the spacing among atoms, which assists in the easy generation
of this passivation layer. These studies also reported that the
formation of this layer with nanocrystallized grains exhibit-
ing higher microhardness, was responsible for the improved
hardness of the cryo-machined surface (Ref 55). As per the
discussion presented in Sect. 3.5, Fig. 17(a) presents the cryo-
milled surface produced by cryo-treated end mill with poor
surface integrity due to the non-uniformly distributed passiva-
tion layer along with surface defects. However, Fig. 17(b)
exhibits hybrid-milled surface with more uniformly distributed
thin passivation layer.
Grain size formed during cryogenic machining is smaller
than that of the grain size formed during other machining
environments (Ref 19). Therefore, the thickness of this
passivation layer may vary with the grain size. In addition,
electrons are more active at the boundaries of finer grains,
which results into the electrochemical reactivity improvement
of the surface. Thus, such a surface promotes a solid
passivation. The firmer association of this passivation layer
with base surface depends on the density of the grain
boundaries (Ref 56). Figure 18 displays hybrid-milled surface
with a 1.21 lm thick and most uniformly distributed passiva-
tion layer. These outcomes display superior performance of
cryo-treated end mill over untreated ones and fall in compliance
with some previously obtained conclusions (Ref 16).
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Fig. 19 (a) Optical microscopic image and (b) FESEM image of cryo-treated end mill used in cryo-milling at 2800 rpm spindle speed and
120 mm/rev feed rate

Fig. 20 (a) Optical microscopic image and (b) FESEM image of cryo-treated end mill used in hybrid-milling at 120 mm/rev feed rate

3.8 Morphological Study of Cryo-treated End Mill
Cutting tool is always expected to display sufficient wear
resistance, toughness, chemical solidity, dimensional stability,
and thermal conductivity against high temperatures and forces
(Ref 13). Figure 19 shows the (a) optical microscopic and (b)
FESEM image of the worn-out cryo-treated end mill. As
discussed and stated in Sect. 3.5, the cryo-treated end mill
demonstrated a more brittle behavior during lowest temperature
milling (cryo-milling). This resulted into its quicker wear at
higher spindle speed and feed rate. The same is evident in
Fig. 14(a) and (b). However, in some studies, the refined grain
structure, higher degree of dimensional stability, and wear
resistance were observed in cryo-treated cutting tools amid wet-
milling (Ref 15). These improved properties could be witnessed
during hybrid-milling, where at the same spindle speed and
feed rate, the cryo-treated end mill got worn out lesser
compared to cryo-milling. The optical microscopic and FESEM
image shown in Fig. 20(a) and (b), respectively, display the
same. This further shows that the temperature of machining
environment can significantly affect the performance of cryo-
treated cutting tools.
4. Conclusions and Scope
The surface defects present on the finally manufactured
degradable biomedical implant or part can cause failure or early
degradation under the joint influence of stress and corrosive
environment. The final significant alteration in the physical,
mechanical, chemical, and metallurgical properties of the part
occurs amid the manufacturing process. Low-temperature
potential machining environments have been proven to achieve
improved surface roughness and microhardness, which further
contribute toward the improvement of corrosion resistance of

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the implant and thus, minimize the chances of implant
loosening and failure.
Based on the experimental findings, the major conclusions
and scope are as follows:
• In the case of milling of Mg alloy AZ31B by untreated
end mill, lowest surface roughness and highest microhard-
ness were obtained during cryo-milling at higher spindle
speed (2800 rpm), lower feed rate (80 mm/rev), and lower
depth of cut (0.5 mm). Higher feed rate and deeper depth
of cut resulted in poor surface roughness and microhard-
ness.
• In the case of milling of Mg alloy AZ31B by cryo-treated
end mill, lowest surface roughness and highest microhard-
ness were obtained during hybrid-milling at higher spindle
speed (2800 rpm), lower feed rate (80 mm/rev), and lower
depth of cut (0.5 mm). Higher feed rate and deeper depth
of cut resulted in poor surface roughness and microhard-
ness.
• In the case of milling of Mg alloy AZ31B by untreated
end mill, oxide (passivation) layer with the lowest thick-
ness and most uniform distribution were observed during
cryo-milling at higher spindle speed (2800 rpm), lower
feed rate (80 mm/rev), and lower depth of cut (0.5 mm).
• In the case of milling of Mg alloy AZ31B by cryo-treated
end mill, oxide layer with lowest thickness and most uni-
form distribution were observed during hybrid-milling at
higher spindle speed (2800 rpm), lower feed rate (80 mm/
rev), and lower depth of cut (0.5 mm). However, the
thickness of the oxide layer obtained in this case was
1.21 lm, which was the lowest thickness among all the
other oxide layer thicknesses observed in this study.
• The performance of cryo-treated end mill seemed to be
dependent on the temperature of the machining environ-
ment. However, further testing would need to be per-
formed to validate the same, which could be one of the
future scopes of the present study.
• The present study designated the different types of surface
cracks (formed on the milled surfaces under the effect of
different input control variable and machining environ-
ments) by visual inspection, based on the grounds of al-
ready reported facts about the machined surfaces of Mg
AZ31B. Hence, this can be experimentally investigated
and verified as another future scope of the present re-
search.
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