Electropolishing SurfaceFinishing
Electropolishing SurfaceFinishing
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Pawan Tyagi1*, Tobias Goulet, Christopher Riso, Kate Klein1, and Francisco Garcia Moreno2
1
Mechanical Engineering, University of the District of Columbia,
4200 Connecticut Avenue NW, Washington, DC, 20008, USA
2
Department of Energy's National Security Campus, managed by Honeywell
14520 Botts Road Kansas City, MO 64147, USA
Corresponding author email: [email protected]
ABSTRACT
Improving surface finishing is the critical step in the application of an additively manufactured
(AM) component. This paper provides insights into the electropolishing route for the surface
improvement of the AM component made up of 316 stainless steel with >6% carbon. We have
discussed the Taguchi design of experiment-based process optimization to understand the role of
various process parameters. Profilometry and scanning electron microscopy were performed to
study the electropolished and unpolished areas of the AM components. Optical profilometry
provided an estimate of the amount of material to be removed to achieve shining and smooth AM
surface. Optical profilometry also provided analysis of several roughness parameters on the
electropolished surface. Electropolishing was effective in reducing the surface roughness below
~0.1 µm RMS. This sub µm RMS roughness makes an AM component suitable for major
engineering applications. SEM showed distinctively different microstructure on the
electropolished surface. We also conducted water contact angle study and spectroscopic
reflectance study on electropolished and unpolished AM component surface. Our study revealed
that electropolishing is a highly promising route for improving the surface finishing of AM
components.
INTRODUCTION:
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engineering component. Higher surface roughness is also found associated with increasing
susceptibility to crack generation, and corrosion [4]. Also, integration of AM part with high
surface roughness in a complex engineering system with multiple components can create
reliability issues. High surface roughness may prevent intimate contact between the component
surfaces and hence lead to loose connections [3] and vibration generation. In addition to the
surface roughness issue, an AM component may have significantly different surface composition
as compared to bulk. Surface finishing is essential to remove the scale from the surface of AM
parts to restore the properties of the bulk material on the surface as well.
However, improving surface finish for an AM component can be very challenging based on
its intricate design [5, 6]. Popular surface finishing approaches like machining, extrude honing,
and sandblasting, may not be applicable for complex AM components [5, 6]. Here we propose
the utilization of electropolishing techniques to improve the surface roughness of metal AM
components. Electropolishing has a unique advantage because it can reduce surface roughness
wherever counter electrode can be placed in the close proximity of target surfaces and electrolyte
solution touches the target surface of a metal AM component [5, 6]. Advantageously, an
electropolishing solution or electrolyte can easily reach intrusions and hidden surfaces which may
be inaccessible by other surface finishing approaches [5]. During electropolishing, the AM
component becomes an anode, and a counter electrode is utilized as cathode[7]. The anode and
cathode are submerged in an acidic electrolyte, and a current is applied. Electropolishing
improves surface finish by removing metal from the surface of a piece, ion by ion [7, 8]. During
electropolishing several improvements commences on AM surfaces: (i) electropolishing
eliminates surface burrs from delicate and intricate AM components. (ii) electropolishing can
effectively improve surface finishing of AM surface by removing scale, oxides, chemicals and
surface irregularities, (iii) electropolishing can make a steel surface corrosion resistance by
eradicating the surface imperfections that serve as corrosion initiation sites, (iv) electropolishing
can significantly improve fatigue life improvement by eliminating micro-cracks and other surface
defects on AM parts, (v) electropolishing can ultraclean AM surface. A number of recent studies
have applied electropolishing on AM components [9-11]. However, there are is limited study on
316 steel with > 6% carbon. Such steel has tendency to form cementite like intermetallic phase.
This iron carbide phase exhibits different physicochemical properties as compared to other
phases present in 316 steel. This 316 steel may be utilized in many critical applications and are
likely to benefit from the AM technology. In this study, we have applied electropolishing based
surface finishing on 316 steel with high carbon content. The efficacy of the electropolishing is
dependent on a number of factors: temperature, agitation, electrolyte composition, and time [7,
12].
Choosing the right combination of electropolishing parameters may be quite challenging
[12]. This paper reports our study to optimize the electropolishing process for the 316 high
carbon steel AM component. We conducted optical profilometry and scanning electron
microscopy (SEM) to quantify the changes surface roughness, and microstructure due to
electropolishing. This paper reports our insights about the electropolishing of the steel AM
component.
EXPERIMENTAL DETAILS
The surface polishing experiments were conducted on the 316 steel AM samples. These
samples were prepared on EOSINT additive manufacturing machine. The 316 stainless steel
2
metal powder was utilized for this study. The powder particle size was > 50 μm. The typical
composition of the finished AM components and the powder was 17-19% chromium, 13-15%
nickel, 6-8% carbon, 2-3% molybdenum, trace elements, and balance iron. The AM components
were produced by direct laser sintering of ~20 μm thick layers.
To investigate the utility of the
electropolishing approach for reducing
surface roughness and improving
surface texture we decided to focus on
four factors: electropolishing time,
temperature, agitation, and electrolyte
composition [7, 12]. To limit the
number of factors and make our
optimization study manageable we fixed
the current density around 80 A/dm2.
However, we separately conducted a
number of experiments to evaluate a
promising current density for the
Taguchi design of experiments. We also
referred to numerous prior studies to
determine suitable current density for
electropolishing on steel AM samples
[6, 7, 12-14]. We utilized Qualitek 4 Figure 2: (a) electropolishing setup. (b) photoresist
software for the design and analysis. A coated AM sample, (c) widows opened in photoresist
L9 Taguchi experimental plan [15] was for electrical contract and electropolishing. (d) An
found suitable to accommodate four electropolished sample.
factors with three levels each (Table 1).
Table 1: L9 Taguchi design of experiment for electropolishing.
1 180 82 X 0
2 180 93 Y 200
4 240 82 X 400
5 240 93 Y 0
7 300 82 Z 200
8 300 93 X 400
9 300 104 Y 0
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To conduct the nine Taguchi experiments we utilized a glass beaker with an acidic electrolyte
(Fig. 2a). Heating and agitation were performed by using a hot plate with a magnetic stirrer
capability (Fig. 2a). In the electrolyte bath, an AM sample and counter electrode were submerged.
To ensure that in all the nine experiments we exposed identical surface area we conducted
lithography on AM samples. Shipley 1813 photoresist was dip coated on AM samples in a class
1000 clean room environment (Fig. 2b). Subsequently, the photoresist coated samples were
heated on the hot plate at 100 °C for 20 minutes. Prolonged baking at high temperature was
accomplished to make photoresist sufficiently hard so that it can withstand acid solution and
other experimental conditions (Fig. 2a). Successively, we opened a ~0.5 cm2 window in the
photoresist shield by selective chemical dissolution of photoresist (Fig. 2c). All the prepared
samples were subjected to electropolishing as per the L9 experimental plan (Table-1). In the
Table-1 X, Y and Z denoted three acid bath composition we utilized. We produced 100 mL
electrolyte solution in water by adding 85% phosphoric acid and 98% sulfuric acid [7, 16]. Other
than water, solution X contained 41 g phosphoric acid and 45 g sulfuric acid, solution Y
contained 49 g phosphoric acid and 41 g sulfuric acid, and solution Z contained 15 g phosphoric
acid and 63 g sulfuric acid. The selection of the electrochemical bath composition was based on
prior literature [5, 6, 12, 13, 16]. After each experiment photoresist was removed from each AM
sample and roughness measurements were performed on the electropolished and unpolished
areas to determine the efficacy of each experiment. For the roughness measurement, the PCE RT
1200 surface profilometer was utilized. Periodically, the roughness meter was calibrated with the
known standard sample. For this study we performed linear scan of 5 mm length. This may be
one of the reason for relatively higher Ra values observed in Taguchi design of experiment.
After conducting the design of the experiment, we also conducted electropolishing on the
cylindrical AM component. The lower part of the cylinder was submerged in the electrolyte bath
and was subjected to electropolishing. The top part was protected by applying the photoresist
insulation coating on the sample surface. After the electropolishing step, the photoresist coating
was removed by submerging the whole sample in the Shipley 1165 photoresist remover. The
optical profilometery was performed with Zeta 20 and Filmetrics optical profilometers to
compare the change in roughness due to electropolishing. We also performed scanning electron
microscopy to study the difference in elemental composition and microstructure before and after
electropolishing.
We have also attempted electropolishing with the optimized parameters on AM steel samples
with internal surfaces. However, only those samples for which we designed the 3D model to
allow the access of a counte electrode in the proximity of target internal surface of AM
component, yielded satisfactory results.
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surface roughness for different samples. For Taguchi analysis we applied “bigger is better”
roughness difference criteria. Invariably, after electropolishing the roughness of each sample
reduced.
Table 2: Roughness measurement on nine samples before and after electropolishing. The last column
shows the difference of sample roughness before and after electropolishing.
Using the experimental data for each run (Table 2) the data analysis was performed.
Initially, we computed the effect of different levels of four parameters (Fig. 3). We calculated the
level total and their averages. To accomplish this objective, results of all trials involving the
particular level of parameters are added, and then divided by the number of data points added.
For instance, for the three levels of time
parameter, the following equations were
adopted [17].
5
The average values of each level of all the parameters were plotted to provide the insight about
their relative impact (Fig. 3). The electropolishing performance kept increasing with temperature
(Fig. 3). However, we are unsure if this trend will continue if one further increases the
temperature. It is expected that secondary processes may interfere. Interestingly, medium level
agitation was found to yield better electropolishing. It is quite likely that higher agitation may
affect the fluid dynamics near AM surface and result in turbulence. The turbulent fluid flow may
interfere with the electrolyte’s electropolishing process. However, medium level agitation is
expected to be good enough to drive away the electropolishing residue from the AM sample
surface (Fig. 3). Taguchi analysis provided clear insight about the electrolyte bath composition.
According to our analysis composition X, which contained 41 g phosphoric acid and 45 g
sulfuric acid, produced the highest
quality electropolishing. Electropolishing
appears to get better with time. We
anticipate that prolonged electropolishing
can gradually reduce the roughness
significantly.
It is noteworthy that Taguchi analysis
is also capable of determining the degree
of interaction among factors [15]. We
made six pairs (4C2) by selecting two
variables at a time using the permutation-
combination rule. Taguchi analysis
ranked the degree of interaction in terms
of % interaction severity index [15]. We
found that time and electrolyte bath
composition were strongly correlated
(Fig. 4). This result can be explained by
noting that electrolyte bath composition
affects the electropolishing rate. Hence, Figure 4: Interaction severity index between two factors.
the amount of electropolishing
accomplished in a given time period is dependent on electrolyte bath composition. We also noted
that agitation and electrolyte bath composition were also correlated (Fig. 4). It seems that efficacy
of one electrolyte composition is strongly related to the agitation. Other factors were also found
to be correlated with another. However, time and agitation were the least correlated (Fig. 4)
To calculate the relative impact of the four parameters, we performed Analysis of variance
(ANOVA) [15]. We calculated the sum of all the results and denoted it by T. The magnitude of T
was found to be 22.525. Subsequently, a correction factor (C.F.) was calculated by dividing the
square of sum by the total number of experiments ( C.F. =T2/9). We computed the sum of squares
(S) by using the following equation: S=T2-C.F. To proceed to the next step sum of squares due to
a parameter were calculated. For instance the sum of squares for the parameter time (A) were
calculated using equation (4).
6
Similarly, the sum of squares for three other parameters temperature (B), composition (C),
and agitation (D) was computed. In the next step error sum of squares (SSe)was calculated by
utilizing the equation (5).
The degree of freedom for all the parameters was calculated. The total degree of freedom was
eight; for each parameter degree of freedom was two (number of levels-1). Subsequently, the
mean square of variance was calculated for different parameters by dividing the sum of squares
with the degree of freedom for the individual parameters. The mean square of variance for the
error was calculated by dividing the SSe with a degree of freedom for the error. Nextly, we
computed the pure sum of square by following the following equation (6)
Similarly, pure sums were calculated for other parameters too (Table 3). Finally contribution (P)
for the individual parameters was calculated by utilzing the following equation.
PA = SS’A/SST. (7)
Similarly, the impacts of the other three parameters were computed and tabulated in Table 3.
Table 3: ANOVA analysis of four parametrs. The last column of the table shows the impact of
individual parameter.
The P values for the individual can be converted into percentage by multiplying by 100.
Taguchi analysis suggested that temperature was the most influential parameter for
electropolishing. The temperature parameter accounted for a contribution of ~40%. The agitation
and electrochemical bath composition were at the second and third place, respectively (Table 3).
The electropolishing period was found to be least influential. In the case of electrochemistry
oxidation and reduction, processes are generally exponentially dependent on temperature [7, 13].
7
Table 4: Elemental analysis in the unpolished and electropolished area.
Chromium 15.1±0.1
Nickel 8.2±0.6
Silicon 1.0±0.6
Nitrogen 2.8±2.0
Sulfur 11.9±0.1
8
electropolishing. This optimum combination of levels for four factors was estimated to give 5.7
μm Ra roughness difference. To cross check this estimation we conducted electropolishing with
the optimized parameters and found that difference in roughness was 4.25 μm (Fig. 2d). We
hypothesize that the small difference between experimentally observed roughness differences as
compared to the predicted one is due to potential variability in the experimental conditions.
Specifically, it may be due to leakage of current through the photoresist insulator, and counter
electrode surface condition, etc.
After determining the suitable combination of electropolishing parameters, we attempted
surface roughness reduction on cylindrically shaped samples. We hypothesized that longer
duration would gradually flatten out high and low sections on the surface of as produced AM
samples. Hence, prolonged electropolishing is expected to yield highly smooth morphology.
Hence cylindrical AM samples were electropolished for ~10 minutes.
We observed that a stainless steel cylindrical sample could be electropolished to yield very
smooth surface roughness. In this study, we are specifically discussing a sample that was
subjected to electropolishing treatment for different periods along its length. The unpolished
section is designated as zone 1, the area with medium electropolishing is designated as the zone
2, and the lowermost section with maximum electropolishing is designated as zone 3 (Fig. 5a).
The prolonged electropolishing with the optimized parameters produced a very smooth surface
(Fig. 5a). The quantitative roughness measurements were performed with Zeta 20 optical
profilometer. Optical images of the zone 3 (smoothest electropolished area) and Zone 1
(unpolished rough area) are shown in Fig.
5b and Fig. 5c. The roughness
measurement was performed in the ~495
µm x 372 µm area.
The smoothest electropolished area
showed ~0.091 µm Ra (Fig. 5d-e) and
unelectropolished area exhibited ~1.88
µm Ra. However, it must be noted that
roughness measurement over a broad
area of the electropolished section
includes many porosities. The 495 µm
long line scan on the electropolished
surface in the smoothest region yielded a
roughness of 0.07 µm Ra. This result
signifies that electropolishing is capable
of achieving the even smoother surface
finish.
Figure. 6. Thickness difference between unpolished
We also investigated the amount of
and electropolished area. (a) Optical microscope
material removal necessary to achieve the
image showing the white color line along which
highly smooth surface finish. To estimate thickness measurement was performed. (b) Etching
the required material removal we depth vs. disctance profile along the white color scan
determined the difference in height for line on image (a). The inset of (b) shows the
the electropolished and unpolished area. difference in hight with respect to unpolished section
The depth profiling was accomplished by plane.
measuring the sample height along a scan
9
traversing from unpolished to the electropolished area (Fig. 6a). The two red color arrows mark
the area where the sharp change in height was determined. The typical difference was around
~200 µm (Fig 7b). This result is critically important in determining the tolerance required to
accommodate electropolishing as the post-processing step. The inset figure shows a cross section
along the scan direction. The back side of 3D view is kept at the unpolished surface height. The
white area in 3D view shows that as one moved from unpolished to polished area, material
removal occurred (Fig. 6b).
We have also electropolished the samples with internal volumes. The internal surface was
not affected by the electropolishing on the AM samples where a counter electrode could not be
placed in the proximity of the internal surfaces. However, outer surface area exhibited
remarkable improvement in the surface finishing due to electropolishing. For the quantitative
analysis, we determined the maximum peak height (Sp), maximum valley depth (Sv), maximum
height difference between peak and valley (Sz), arithmetic mean height (Sa), and root mean square
(RMS) of height (Sq). The surface skewness factor (Ssk) and surface kurtosis (Sku) were also
determined. We recorded these roughness parameters in 0.2 x 0.17 mm2 area on eight different
locations. The magnitude (Sp) was 166.35±18.65 µm for the unpolished AM surface which was
reduced to 16.38±6.65 µm for the electropolished AM samples. Similarly, the depth of valley (Sv)
was 60.12±20.10 µm for the AM surface before electropolishing. After electropolishing Sv
reduced to 28.12±8.31 µm. The difference between the height of the tallest peak and deepest
valley (Sz) for the AM sample before electropolishing was 226.44±17.67 µm. After
electropolishing Sz reduced to 44.50±13.45 µm. The surface roughness parameter (Sa) for the
unpolished surface was 13.88±2.65 µm. After electropolishing Sa reduced to 3.0±0.75 µm. The
RMS roughness (Sq) for the unpolished AM surface was determined to be 17.37±3.02 µm. After
electropolishing Sq decreased to 3.77±0.85
µm. The surface skewness factor (Ssk)
magnitude was 0.10±0.98 for the unpolished
surface, which indicates that the number of
hills and valleys are almost in the same
proportion to one another. However, Ssk
parameter became negative for the
electropolished samples indicating the
dominance of cavities. Ssk was -0.29±0.85
for the electropolished sample. The surface
kurtosis (Sku) describes the peakedness of
the surface topography. If Sku=3, then the
distribution is ideal Gaussian-like. Sku was
calculated for the whole area and determined
to be 2.2 for the unpolished AM sample and
3.4 for the electropolished. This data
indicates that a electropolished sample was
significantly biased towards having a higher
Figure. 7. SEM images from the zone 1 and zone 3. (a,
proportional number of valleys. We also c) Images from electropolished area at various
found that electropolishing can be magnification. (b and d). Images from the unpolished
performed on the internal volume of the AM area at various magnifications.
steel components by considering the counter
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Figure. 8. SEM images obtained using backscattering detector from (a) optimally electropolished 316 AM
sample and (b) from excessively electropolished AM sample.
electrode access during the design stage. We prepared cubic AM samples with ~1 cm diameter
holes to allow counter electrode to easily enter into the internal volume. Electropolishing
effectively reduced the surface roughness of the internal volume. Hence, one can design an AM
component by considering the needs of electropolishing in mind.
We also performed scanning electron microscopy (SEM) to investigate the difference in
composition and microstructure of the electropolished and unpolished area. The Electron
Dispersive Spectra (EDS) study showed that surface composition was entirely different and
contained high oxygen content. Interestingly, after the removal of ~ 200 µm, thick material from
the surface during electropolishing yielded typical stainless steel composition. The composition
of the electropolished area was akin to the composition of stainless powder utilized for the AM.
It is noteworthy the unpolished surface (Fig.7a) was gray in color and signified the change in
composition. The typical steel surface is shiny and has silver color as shown in the
electropolished area (Fig. 5). This result is of critical importance when welding of the AM
component of other parts is important. Also, physio-chemical properties of the unpolished
surface will be entirely different as compared to the stainless steel surface.
The microstructure of the electropolished and unpolished surface was expected to be quite
different. We performed SEM study and found that at high magnification the electropolished
surface was predominantly featureless (Fig. 7a), as compared to the unpolished area (Fig. 7b).
The unpolished section on the AM produced cylinder contained the flaky pattern. At medium
magnification, the electropolished surface appeared featureless. However, setting the SEM
parameters to yield higher contrast revealed various microstructural features (Fig. 7c). On the
other hand the unpolished section at the same magnification still, exhibited a flaky pattern (Fig.
7d).
We also utilized back scattering dtector of the SEM to study the electropolished AM samples.
We found that an optimally electropolished 316 AM sample yielded quite regular micorstructure
11
with numerous pits or cavities. Overall surface is quite smooth and exhibited ~0.5 µm roughness
(Fig. 8a). It is noteworthy that Fig.8a also contain sub-micron garins which are faintly observable
in Fig.8a. However, Fig.7d provide a
better contrast. We became interested in
investigating if we could etch away the
pits or cavities seen in the Fig.7d and
Fig.8a. For that we conducted
electropolishing for the extended period
and studied the 316 AM steel sample with
the back scattering detector of the SEM.
The microstructure of the excessively
electropolished AM sample turned out to
be significantly different (Fig. 8b). As
seen in the SEM image the several pits
area started to disappear, but several
continued to persist (Fig.8b). This study
suggest that pits or cavities observed after Figure 9: Reflectance characteristics of the
electropolishing possessed different electropolished and unpolished (rough) surface of an AM
depth. Interestingly, excessively steel component.
electropolished sample showed very clear
presense of near hexagonal grains (Fig.8b). The small hexagonal grains contain rather smooth or
flat interior regions but the grain booundary region is significantly etched. It appears that grain
bounday region is more suceptible to etching as compared to interior region of the grains. We
surmise that at the grain boundarry cementite phase was expected to be present for the high
carbon 316 steel grade as used in this study. Presumably, the cementite along the grain
booundaries etched away faster than the low carbon phase present within the interior of the grain.
12
We also studied the difference in the surface chemistry of the unpolished and
electropolished AM samples. For the study of surface chemical properties, we utilized water
contact angle measurement. In this experiment ~100 µL water drop was introduced on cleaned
and dried AM sample surfaces. The unpolished 316 AM steel sample formed ~90° angle at the
junction of water, AM surface, and air (Fig. 10a). However, the electropolished AM sample yielded
~45° contact angle. The smaller contact angle indicates that the electropolished sample became
significantly hydrophilic, as compared to the unpolished AM sample. Further study by XPS like sensitive
surface measurement may provide more profound insights about the surface chemistry of electropolished
samples.
CONCLUSIONS
In this paper, we demonstrated the utilization of the electropolishing approach to improving
the surface finish of as produced 316 high carbon stainless steel metal additive manufacturing
components. To systematically understand the impact of electropolishing factors such as
temperature, agitation, electrolyte bath composition, and time we have employed the Taguchi
design of experiment approach. We conducted parameter optimization on the rectangular
samples. The results of Taguchi design of experiments were implemented on cylindrical shaped
AM samples. Electropolishing with optimized parameters could drastically improve the surface
finish of the AM components. The typical surface roughness decreased below ~0.1 µm Ra.
Electropolishing also removed the scale from the AM component surface and brought out the
surface with typical stainless-steel composition and bright luster. The electropolished surface
possessed a significantly smaller defect population on the AM surface. We also found that nearly
~250 µm thick material should be removed during electropolishing to attain highly smooth
surface finish. Scanning electron microscope imaging revealed that as produced AM steel
component had flaky morphology, along with pits like features. The microstructure of the
electropolished surface was dramatically better than that of as produced AM surface.
Electropolishing was effective in improving surface finishing of AM component if a counter
electrode could be placed in the close proximity of the AM component.
ACKNOWLEDGMENTS
We gratefully acknowledge the funding support from the Department of Energy-National
Nuclear Security Agency (Subaward No. 0007701-1000043016). This work is in part supported by the
Department of Energy’s Kansas City National Security Campus. The Department of Energy’s Kansas
City National Security Campus is operated and managed by Honeywell Federal Manufacturing &
Technologies, LLC under contract number DE-NA0002839. We also thank Sebastian and Matt Jobins of
Nanoscience Instrument for the assistance with SEM imaging. We appreciate assistance from Jim Elmen
of Filmetrics for optical profilometry.
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