Journal of Alloys and Compounds 804 (2019) 84e92

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

The effect of residual stresses, grain size, grain orientation, and

hardness on the surface quality of CoeCr L605 alloy in Photochemical
Machining
Shrikant Thorat*, Mudigonda Sadaiah**
Department of Mechanical Engineering, Dr. Babasaheb Ambedkar Technological University, Lonere, Raigad, Maharashtra, 402 103, India

a r t i c l e i n f o a b s t r a c t

Article history: This paper presents the study of surface integrity of CoeCr alloy in Photochemical machining (PCM). The
Received 13 March 2019 surfaces were selected from different manufacturing processes such as forged, machined and, rolled. The
Received in revised form responses such as surface roughness (Ra) and depth of etch were studied in correlation with PCM process
26 June 2019
parameters like etching temperature for a constant time and concentration. Further, characterization
Accepted 27 June 2019
techniques viz. XRD, EBSD, hardness test and SEM were employed to evaluate residual stresses, grain
Available online 28 June 2019
size, grain orientation, hardness, local intergranular misorientation, and surface topography of the CoeCr
L605 alloy. These metallurgical parameters were corroborated with experimental results. The order of Ra
Keywords:
PCM
and depth of etch for three conditions are: forged > machined > rolled.
CoeCr L605 © 2019 Elsevier B.V. All rights reserved.
Metallurgical aspects
Surface roughness
Depth of etch

1. Introduction bioimplants and surgical tool applications. Therefore, bioimplants

including orthopaedic, cardiovascular, and dental require a Ra value
CoeCr L605 is a superalloy which emergently used in the field of in the range of 10 nme100 mm to enhance the biocompatibility and
aerospace, marine, energy, food, chemical, and bio-medical in- performance [8].
dustries, because it combines the inherent corrosion resistance, Different manufacturing techniques were used to create several
outstanding mechanical strength, excellent fatigue strength and surface topographies and surface configurations. These are divided
bio-compatibility. By virtue of this, it is most suitable for into mechanical, chemical, electrochemical, electropolishing, vac-
manufacturing of bio-implants and surgical instruments viz. stent, uum, and thermal and laser. The chemical etching method might be
heart valves, bone and joint replacements, dental braces, bridges, suitable to create micro-topography over a surface of bio-implants.
dentures, blades and scalpels [1e6]. Owing to the controlled surface oxides formation helps to provide
Over recent years, the in vitro and in vivo study for biocom- better bonding between bones to the implant which improves
patibility of bio-implants exhibits a need for Osseointegration tissue growth [9e11]. PCM is a chemical machining process used to
process. The Osseointegration is a direct and stable growth of bone create microtextures and components at lower cost. Recent inves-
tissue over surfaces of the implants. Surface textures have abilities tigation shows the resurgence of the PCM process. It has been
for the augmented growth of bone tissue in perspective integration employed to manufacture interdisciplinary applications viz. medi-
and adhesion of tissue to bone [7]. Surface topography of implants cal devices, biotechnology, micro-reactors, lab-on-a-chip, elec-
plays a significant role in the development of bone-implant contact tronic components, communication technology and jewellery.
with an increased growth rate of tissue. However, the surface Concurrently, it is focused on the machining of material such as
roughness values are dependent upon the according to the Inconel 718, Monel 400, Brass, SS316L, Cu, SS304, German silver
[12e18].
The surface integrity of CoeCr L605 has not been studied in the
* Corresponding author. extension of bio-medical application. The present study focuses on
** Corresponding author. to investigate the link between metallurgical aspects and surface
E-mail addresses: [email protected] (S. Thorat), msadaiah@dbatu. topography using PCM for the bio-engineering applications.
ac.in (M. Sadaiah).

https://doi.org/10.1016/j.jallcom.2019.06.358
0925-8388/© 2019 Elsevier B.V. All rights reserved.
 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92 85

Table 1
Material characterization of CoeCr L605 alloy.

Elements Co Cr W Ni Fe Si Mn Mo P Se

% wt 52.10 18.46 13.38 8.61 1.32 3.66 2.02 0.007 0.8 0.25

Fig. 3. Effect of manufacturing processes on surface roughness.

the surface. Lamination carried out immediately after preparation

Fig. 1. Specimen of CoeCr L605 used in the experiment. of the sample, over the polished surface by a flow coating method. A
CAD software was used to prepare photo tool for exposing over the
laminated surface. In exposing, the ultraviolet (UV) light was
2. Materials and methods exposed over a photo tool to transfer the artwork on the laminated
surface. It is followed by a developing process. In this, a developer
Due to a wide range of applications in the biomedical field, the solution was used to develop the artwork. The artwork was
CoeCr L605 alloy has been selected for the experimental study. The developed by retaining photopolymer, and the remaining was weak
chemical composition of CoeCr L605 alloy is given in Table 1. Ex- which dissolved in the developer. After that, post-baking was car-
periments were conducted on specimen size of 20 x 8
0.5 mm flat ried out, to harden the remained photoresist film. And finally, wet
sheets of Coe Cr L605 with a channel of 10
2 mm of width was dip etching was performed using a hot plate with a magnetic stirrer,
etched on the surface, shown in Fig. 1. the schematic representation shown in Fig. 2.
Typically, the PCM process was carried out in two steps, i.e. From the literature survey [4], and preliminary experiments, a
sample preparation and wet corrosion of the metal in a controlled specific etchant has been selected for PCM of CoeCr L605. It con-
manner. Prior to experiments, the sample preparation was carried sists of etching agent, a reducing agent, and an oxidizing agent in an
out using ultrasonic cleaning process. It was used to remove the alkaline solvent; It is the mixture of FeCl3 (Ferric Chloride), HCl
dust, rust, and oil particles from the surface without changing the (hydrochloric acid), and H2SO4 (sulphuric acid) in a CH3OH
surface topography. The contaminated surfaces become a barrier to (methanol) whereas, they are mixed by percentage weight of 0.09,
the etching process. It would impede the uniform chemical etching. 0.13, 0.26, and 0.52 respectively. The etching process was carried
A photoresist is a UV sensitive thin polymer layer applied to coat out at a constant temperature of 30  C for 50 min.

Fig. 2. Experimental set-up for PCM of CoeCr L605 alloy.

86 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92

Fig. 4. Surface roughness of the CoeCr L605 for before etching: (a) rolling, (b) milling, (c) forging and after etching: (d) rolling, (e) milling, and (f) forging.

The input parameters viz. etchant concentration, etchant tem- grain orientation, hardness [19], and etched surface topography of
perature and time of etching have been studied for the influence of the CoeCr L605 alloy to corroborate the surface quality.
surface roughness, and depth of etching. Whereas, the post process
comprises the measurement of depth of etch, etch rate, and surface 3. Results and discussion
roughness and inspection of the surface. The optical 3D surface
profilometer: Alicona and Veeco were used to measure the depth of 3.1. Effect of manufacturing processes on surface roughness
etch and surface roughness. However, etch rate is calculated from
the ratio of the depth of etch to the time required to etch. The three manufacturing processes viz. forging, milling, and
Furthermore, characterization techniques viz. XRD, EBSD, hardness rolling were employed to prepare the workpiece of the required
test and SEM were used to evaluate residual stresses, grain size, dimensions (thickness 0.5 mm). The optimum parameters were

Fig. 5. XRD analysis of an etched microchannel of the forged sample at f ¼ 180 .

 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92 87

Fig. 6. XRD analysis of an etched microchannel of the milled sample at f ¼ 180 .

selected for each process [20]. These processes change the micro- 3.2. Effect of residual stresses
structure and surface topography of the CoeCr L605 due to their
influential parameters. Fig. 3 showed that the effect of different Figs. 5e7 illustrates XRD analysis of etched microchannel of
manufacturing processes on Ra using PCM. The primary Ra values samples, which are prepared by three different manufacturing
(before etching) were obtained 5.07, 2.16, and 0.952 mm for forging, processes such as forging, milling, and, rolling to reduce the
milling, and rolling, respectively. The Ra values (after etching) were thickness to 0.5 mm. The XRD analysis of the forged sample is
found to be 1.69, 1.01, and 0.582 mm for the order mentioned above, shown in Fig. 5. The result shows maximum stress is 912.7 MPa in
and it is shown in Fig. 4. The obtained values are improved than X-direction. The residual stress generated is a positive magnitude
primary values. The heat generation and applied forces alter the which indicates that tensile residual stress. Whereas, the initial
surface properties by imparting the residual stresses, hardness, and value of the residual stress is 813.6 MPa present in the sample
different grain growth rate, which causes variation in Ra value for which was rolled. In comparison with other manufacturing pro-
the different manufacturing processes. cesses, the forging induces maximum tensile residual stresses
which were corroborated by Fig. 5. The depth of etch is obtained for
the forged sample is 55.01 mm. It is the maximum depth of etch

Fig. 7. XRD analysis of an etched microchannel of the rolled sample at f ¼ 180 .

88 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92

Fig. 7 depicts the XRD analysis of the rolled sample. Fig. 6 clearly
shows the negative slope of the graph; it indicates that the induced
residual stresses are compressive along the X direction. The
magnitude is 813.6 MPa. In this condition, the depth of etch rate is
found to be 18.25 mm. In first both cases, tensile residual stresses
were induced. The samples were elongated along X-direction. The
d spacing, i.e. interplanar distance for forged and machined sam-
ples were 1.2630 Å, and 1.2635 Å obtained respectively. But, the
rolled sample induced by compressive residual stress along X-di-
rection, in this d spacing increased to 1.26667 Å. In tensile stresses,
etch rate is maximum due to an occurrence of three phenomenon;
i) reduced interplanar distance, ii) increase in atomic distance and
iii) decreased grain size [21].
However, residual stresses affect the crystal structure, inter-
Fig. 8. Effect of manufacturing processes on the hardness. planar distance, and interatomic distance. According to Bragg's law
[22], as predicted in equation (1),

achieved in comparison with three manufacturing conditions. nl ¼ 2dsinq (1)

Fig. 6 depicts the XRD analysis of etched microchannel of the
machined sample. The residual stress generated in this case is Where n is the number of rays, l is the wavelength of the x-ray,
278.7 MPa and almost half of the forged sample. The maximum d is the interplanar distance, and q is the diffraction angle. The
depth of etch is 42.7 mm, and etch rate decreased by 22%. It explains grains that have planes of atoms with an interplanar distance. The
the relationship between the magnitude and direction of residual grains that have planes with this spacing which are parallel to the
stress and the etch rate of the material. surface will diffract. This diffraction takes place from a thin surface
layer. If the surface of the sample is in compression, the ‘d’ spacing

Fig. 9. EBSD images of rolled (annealed) specimen: (a) Grain size (b) grain orientation (c) Grain area fraction.
 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92 89

Fig. 10. EBSD images of milled specimen: (a) Grain size (b) grain orientation (c) Grain area fraction.

of these planes is larger than in the unstressed state, because of the Whereas TS is tensile stress, H is the hardness, and n is the
Poisson's effect. On tilting the sample, new grains diffract, and strain-hardening exponent. From equation (3), it is clear that
orientation of the diffraction planes is more nearly perpendicular to hardness significantly affects the tensile stress. Also, the increase in
stress direction. the hardness increases the strain hardening rate. Hence, the infla-
In contrast, for tensile residual stresses, the ‘d’ spacing of these tion in strain-hardening rate and hardness increases the tensile
planes are smaller than unstressed state. Because of this, it de- stress in the material. In addition to this, hardness was the conse-
creases the distance between the atomic planes; it increases the quence of lowered grain size. This increases the total interface
linear atomic density. And simultaneously, increases the distance volume, which is the volume of grain boundaries and triple junc-
between atoms which leads to in weakening of the atomic bonds. tion. The triple junction is the weakest region of the surface. The
Consequently, it increases the etch rate. triple junction was comprised with lower density, uneven and
different coordination atoms (atomic defects), segregation of the
3.3. Effect of hardness impurities, and different charge of atoms. Due to this, mass diffu-
sion was uncontrollable which increases the etch rate.
The hardness of the samples was determined according to IS
1501 test using Vickers hardness tester (VM-50PC, FIE). Each sam-
ple was measured under the micro Vickers hardness test, Hv 0.5 3.4. Effect of grain size and grain orientation
loading condition of 0.1961 test force (N) with three trials. The
average hardness of three trials such as H1, H2, and H3 for rolled, Contextual to the metallurgy of CoeCr L605 in PCM, the grain
milled, and forged sample was found to be 264, 424, and 506 Hv size and their orientation largely affect the PCM process. EBSD
respectively, as shown in Fig. 8. Substantially, the hardness of the (Electron Back Scatter Diffraction) microscopy provides informa-
material influences the etches rate in PCM. Because, according to tion about grain size, grain orientation, and local intergranular
the Hall-Petch relationship, the hardness was a relation with stress- misorientation. The effects of grain size and grain orientation on
induced, elastic modulus, grain size, and interatomic spacing [23]. corrosion behaviour of CoeCr L605 alloy were analyzed. The output
According to Cahoon et al. [24], as shown in equation (2), such as surface quality and etch rate were affected.
Substantially, it affects the PCM process regarding depth of


H n n etching, etches rate, and surface quality. Fig. 9. 10, and 11illustrate
TS ¼ (2) the grain size and grain orientation were from EBSD plot for rolled,
2:9 0:217
milled, and forged respectively. The maximum grain size was found
90 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92

Fig. 11. EBSD images of forged specimen: (a) Grain size (b) grain orientation (c) Grain area fraction.

to be 122 mm for rolling whereas it was obtained 97.6 mm and 27 mm the more dislocations were present at grain and the greater the
for milling, and forging, respectively. The etch rate was obtained stress-field transpired at grain boundaries. The cumulative effect of
0.37, 0.85, and 1.1 mm/min for rolled, milled, and forged, respec- these factors susceptible the material to increase the etch rate.
tively. The results showed that the grain size has an inverse relation Fundamentally, grain boundaries are the interface of the grains.
with etch rate. According to the Hall-Petch equation (3), It is a region, where maximum atomic disarray occurs at which
faults and dislocations congregate. This disarray brings out ener-
k getically at ease for impurities to concentrate at grain boundaries in
sy ¼ so þ pyffiffiffi (3)
contrast with grain interior due to more regular arrangements. The
d
areas at which these defects emerged over the surface constituent
Where sy is yield stress, so is material constant for starting stress with high activation energy, it prone the material in increasing
(resistance of the lattice to the dislocation movement), ky is chemical affinity [1]. The stability or variation in Ra is mainly
strengthening coefficient, and d is the grain diameter. The equation dependent upon the diffusion reaction of CoeCr L605 and etchant.
(3) corroborates the obtained etch rate. Simultaneously, grain However, the diffusion rate is directly proportional to the grain size
orientation decides the direction of the stress-field vector. From of the material. In case of larger grain size, the Ra is low compared
Fig. 9 (rolled), the orientation of grain was uniform. Where in the to smaller grain size at the same time [13]. Whereas, the rolled
forged sample (Fig. 11) the highly random orientation of the grains sample has a larger grain size than machined which was greater
are present. This varies the direction of stress-vector at every grain than forged.
boundaries, which weaken the surface of the material.
The presence of stress imparts dislocations in the crystal
3.5. Effect of local grain misorientation
structure. The dislocations create stress-field around it, and is given
by Ref. [25], as predicted in equation (4),
In this context, effect of local inter-granular misorientation was
studied in the PCM of CoeCr L605 to explore the surface topog-
Gb
s¼ (4) raphy. Fig. 12(a), (b), and (c) showed the influence of different
r manufacturing processes on the orientation of grains with respect
Where s is stress, G is shear modulus, b is the Burger vector to each other, whereas, it is found to be 25.83 , 38.06 , and 48.54
(magnitude and direction of lattice direction), and r is the stress- average misorientation for angles for rolling, milling, forging,
field distance from dislocations. The dislocations movement were respectively. From Fig. 12(a), it is seen that the maximum grains are
occurred along the grain and across the grain boundaries. Hence, laid at 2.5 , whereas more than 60% grains area is found to be below
 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92 91

30 . The local inter-granular misorientation for milled (Fig. 12(b))

shows that 45% grain area is below 30 and remaining spread over
the 30 e60 . Sequentially, for the forged sample (Fig. 12(c)), the
maximum grain area is found to be at 60 , and almost 75% grain
area spread over the 30 angles. However, the Read and Shockley
theory [26] predicts that the increase in grain boundary energy
with a misorientation angle of grain. The misorientation angle has a
considerable impact on the etching. The grain boundary energy is
mainly dependent on the grain misorientation angle of the grains.
The consequences of the grain misorientation impart high dislo-
cations which inflate the chemical activation energy of the grains;
which result rise in chemical affinity of the material. In CoeCr L605;
the Fig. 12(a) depict maximum grain misorientation of less than 5 .
Hence free grain boundary energy is low. Therefore, chemical
activation energy at the grain boundary is low, which shows that
CoeCr alloy has a low tendency for chemical affinity and hence
lower etch rate. Conversely, milling and forging processes seizures
average higher misorientation angle is more than 30, which leads
to a higher etch rate.
Fig. 13(a) shows SEM of an etched surface of the forged sample,
whereas Fig. 13(b) and (c) shows the SEM image of the milled, and
rolled, respectively. The image shows better surface topography in
rolled as comparatively to the forged. The etch rate was obtained
0.37 mm/min, with a better-quality surface finish of 0.582 mm. This
is due to the combined effect of residual compressive stress, lower
grain misorientation angle, optimum hardness, and higher grain
size of the material. It results in a lower etch rate. This advances the
reaction smoothly; that is, the etching process was completed with
the removal of atoms by a plane-by-plane, with continuous and
progressive etching. This is due to the existence of lower chemical
affinity. In contrast, milled and forged surfaces have more Ra and
depth of etching. Substantially, the surface roughness plays a sig-
nificant role in the osseointegration and fatigue life of bio-implants.
The rolled sample can be used as raw material for bio-implant
manufacturing. The manifestation of compressive residual
stresses, large grain size, optimum hardness, and minimum local
grain misorientation helps to reduce localized corrosion over the
bio-implant surfaces.

4. Conclusions

The investigation of PCM of CoeCr L605 is carried out to study

the surface topography. The experimental study is significantly
concluded as follows:

 The Ra and etch rates were found to be 1.69 mm, 1.01 mm, and
0.582 mm, of 0.37 mm/min, 0.85 mm/min, and 1.1 mm/min for
rolling, milling, and forging, respectively.
 The results were obtained for residual stresses of 912.7, 278,
and 813.6 MPa in the X-direction for forged, milled, and rolled
workpieces, respectively. Furthermore, tensile residual stresses
enhance the etching rate; whereas, the compressive residual
stresses lower the etch rate. However, it increases surface finish.
 It was observed that grain size is inversely proportional to the
surface roughness, due to the difference in grain boundaries.
 Substantially, the grain orientation is influences the depth of
Fig. 12. Fractions of grain area with grain misorientation in parent metal for the etched etching and Ra. The grains of the rolled surface has maximum
sample. (a) Grain misorientation of the rolled sample, (b) Grain misorientation of and uniform orientation along (001) plane i. e. the atoms were
milled sample, and (c) Grain misorientation of forged sample.
present over the surface have a similar energy level, whereas, in
case of milling and forged surface grains were arbitrarily
oriented.
 The local intergranular misorientation angle influences the PCM
process, and the average misorientation angles were found to be
25.83 , 38.05 , and 48.54 for rolling, milling and forging,
respectively.
92 S. Thorat, M. Sadaiah / Journal of Alloys and Compounds 804 (2019) 84e92

Fig. 13. SEM image of microchannel etched: (a) forged, (b) milled, and (c) rolled sample.

 Substantially, hardness considerably affects the etch rate. It etching solution for nickel-chromium-beryllium and chromium-cobalt alloys,
J. Prosthet. Dent 62 (5) (1989) 516e521.
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