metals

Article
Characterization of Magnetoelectropolished Stainless
Steel Surfaces’ Texture by Using the Angle-Resolved
Scattering and Image Processing Analysis Methods
Wojciech Kapłonek 1 , Krzysztof Rokosz 2, * and Danil Yurievich Pimenov 3
1 Department of Production Engineering, Faculty of Mechanical Engineering, Koszalin University of
Technology, Racławicka 15-17, 75-620 Koszalin, Poland; [email protected]
2 Department of Engineering and Informatics Systems, Faculty of Mechanical Engineering, Koszalin
University of Technology, Racławicka 15-17, 75-620 Koszalin, Poland
3 Department of Automated Mechanical Engineering, South Ural State University, Lenin Prosp. 76,
454080 Chelyabinsk, Russia; [email protected]
* Correspondence: [email protected]; Tel.: +48-943478354




Received: 21 July 2020; Accepted: 11 August 2020; Published: 13 August 2020


Abstract: In this article, the results of preliminary experimental studies related to a fast, non-contact
assessment of the AISI 316L stainless austenitic steel surfaces after electrochemical polishing in a
magnetic field have been presented. The experiments were realized with the use of a modified
angle-resolved scattering (ARS) method based on the analysis of angular distribution of the scattered
light intensity. Digital images of such distribution were acquired for selected areas of examined
samples—base surface and surface after magnetoelectropolishing (MEP) process. Parametric analysis
oriented toward the calculation of selected key geo- and photometric parameters carried out in
Image Pro® -Plus software allowed for characterization of the surface conditions of the assessed
samples in terms of their scattering properties. The obtained experimental results confirmed the
usefulness of the ARS method used in the presented studies as well as the possibility of its practical
use (after appropriate modifications) on a wider scale, especially in industrial applications.

Keywords: magnetoelectropolishing; stainless steel; non-contact methods; angle-resolved scattering;

image processing and analysis

1. Introduction
At the beginning of the twentieth century, the production of austenitic stainless steels for application
in the chemical, energy and food industries was introduced. The continuation of the research in the
early 1970s allowed for the improvement of the existing methods thanks to the application of new
refining and casting processes. It has to be pointed out that the addition of nickel (8–23%) and/or copper
(0.2–0.75%) and/or manganese (0.3–4%) is necessary to obtain the austenite structure. Other elements,
such as carbon (0.02–0.08%), chromium (17–28%), molybdenum (2–8%) and nitrogen (0.1–0.6%),
have a significant influence on both the mechanical properties and the corrosion resistance. The yield
(170–500 MPa) and tensile (214–795 MPa) strengths are obtained mainly by addition of carbon and
nitrogen [1]. In addition, they cannot be hardened by heat treatment, so they are cold-worked by
forming, spinning and swaging, which increase their strength. Electrochemical polishing processes are
used to reduce the surface roughness as well as to form on the top of surface the chromium enriched
nano-layer, which has better corrosion resistance than the air-oxidized matrix [2,3].

Metals 2020, 10, 1098; doi:10.3390/met10081098 www.mdpi.com/journal/metals

Metals 2020, 10, 1098 2 of 15

The first mentions of electrochemical polishing (EP) date back to 1912, when the German
government issued a patent for silver finishing [4]. The next milestone was Jacquet’s work on polishing
copper in phosphoric acid H3 PO4 [5], followed by the work of, among others, Elmore [6], Wagner [7],
Hoar [8] and Hensel [9]. The subsequent studies by Landolt showed that the double layer consists of
three sublayers: the first is a semiconductor type with a metal surface 10–11 nm thick, the second is a
discontinuous layer of metal ions subject to digestion, and the third is a diffusion layer much thicker
than the previous two [10]. The proposal of a discontinuous layer of metal ions is a good solution;
however, it should be considered that this liquid layer may also contain anions derived from the
electrolyte or complexes containing water molecules, which the author of the article does not analyze.
Kirchheim et al. [11] considered the change in current density with time on the basis of Fick’s second
law, distinguishing three phases of EP. They noticed that, in the first phase of the process, the current
density is approximately constant over time; then, in the second phase, it decreases, which may be due
to the formation of a permanent film of reaction products on the anode; it then reaches a constant level
again due to natural or forced convection in the case of long-term polishing and/or mixing the solution.
The presented theory assumes the mass transport mechanism in the layer in all three phases of EP
diffusion. An analysis of the literature shows that, in the EP process at the metal–solution interface,
complex processes take place, the explanation of which may be based on various models. The models
have a common feature—the division into layers, the outer ones being more enriched with ions from
the solution, and the inner ones with cations of the metals of the base. The concept of Grimm et al. [12]
was based on three layers: the internal compact salt oxide enriched with alloy metal cations (substrate),
which turns into a porous/semi-liquid composed of hydrated salts, complexes with a negative total
charge and anions derived from the electrolyte and external diffusion.
Currently, research on the process of standard EP [13,14] is still being carried out, an example of
which is a better description of the treated surfaces in terms of chemical composition [15,16], hydration
of the top layer [17] and surface roughness [18,19], corrosion resistance [20,21] as well as reduced
Young’s modulus and nanohardness [22]. The latest research concerns magnetoleltoctopolishing
(MEP) [15–17] and polishing with the use of very high densities (1000 A/dm2 ) [23,24].
The effectiveness and correctness of the EP and other polishing processes can be verified using a
number of advanced observation measurement methods, presented, among others, by Pahk et al. [25],
Duparré [26] as well as Rebeggiani and Rosén [27]. Since the obtained surface is smooth, with small
heights of surface irregularities, and additionally is characterized by a low resistance to pollution,
susceptible to deformation and sensitive to physical or chemical effects, the use of non-contact methods
is most advantageous in this case. These include high-accuracy variations of microinterference methods
(e.g., phase shifting interferometry (PSI)), advanced optical microscopy (e.g., confocal laser scanning
microscopy (CLSM), focus variation microscopy (FVM)) and high-resolution electron microscopy
(e.g., scanning electron microscopy (SEM)) as well as scanning probe microscopy (e.g., atomic force
microscopy (AFM)). An interesting group of such methods are also those which are based on the
imaging and analysis of scattered light. The characteristics of the abovementioned methods in
relation to their resolution (vertical and lateral) and observation measurement ranges are presented
schematically in Figure 1.
Metals 2020, 10, 1098 3 of 15
Metals 2020, 10, x FOR PEER REVIEW 3 of 15

Figure
Figure1.1.Approximate
Approximateresolution
resolutionranges
ranges(horizontal
(horizontaland
andlateral)
lateral)characterizing
characterizingthe
themodern
modernadvanced
advanced
observation
observation measuring non-contact methods used for assessment of surfaces after the
measuring non-contact methods used for assessment of surfaces after the polishing
polishing
processes,
processes,modified
modified based
based on
on [28].
[28].

One
One ofof the
the light-scattering
light-scattering methods
methods isis angle-resolved
angle-resolved scattering
scattering (ARS),
(ARS), widely
widely presented
presented by by
Azarova at al. [29], Bloomstein et al. [30], Schröder et al. [31], Zhenrong et al. [32] as
Azarova at al. [29], Bloomstein et al. [30], Schröder et al. [31], Zhenrong et al. [32] as well as Kapłonek well as Kapłonek
and
andNadolny
Nadolny[33]. [33]. This
Thismethod
methoduses usesthe
themeasurement
measurementof ofthe
theangular
angulardistribution
distributionof ofscattered
scatteredlight
light
intensity.
intensity. Its
Itstheoretical
theoreticalbasis
basiswas wasformulated
formulatedinin1967
1967by byTorrance
Torranceand andSparrow
Sparrow[34].[34]. InInTorrance–
Torrance–
Sparrow
Sparrow(T-S)
(T-S) theory,
theory, as a model
model of of scattering
scattering surface,
surface, aa mirror
mirror facet
facet model
model (MFM)
(MFM) is is used.
used. TheTheARS
ARS
method
methodcomes
comesin in many
many variants
variantsand and varieties,
varieties,which
whichallows
allowsfor for flexible
flexible selection
selectionof of resolution
resolution and
and
measuring range for a given application. Due to the relatively wide range of
measuring range for a given application. Due to the relatively wide range of resolutions offered, resolutions offered, the
ARS method
the ARS method is basically used
is basically usedin applications,
in applications,in in
which
which thethemeasured
measuredsurfaces
surfacesare arecharacterized
characterizedby by
the
thefollowing:
following:
• relatively low heights of irregularities from approx. 0.2 to 200–300 nm (optical and opto-
• electronical
relatively low heightssilicon
elements, of irregularities fromimplants
wafers, tooth approx. and0.2 toartificial
200–300hip nmjoint
(optical and opto-electronical
prosthesis stem balls),
elements, silicon wafers, tooth implants and artificial hip joint
• high heights of irregularities from approx. 500 to 1500–2000 nm (precisely machined prosthesis stem balls), machine
• parts,
high automotive
heights of irregularities
components,from approx.
medical 500elements
devices to 1500–2000 nm (precisely
and parts machined
of aeronautical machine
engines).
parts, automotive components, medical devices elements and parts of aeronautical
The assessment of the surface texture after the EP and other polishing processes requires the engines).
application of the first of the mentioned varieties of the ARS, as reported Łukianowicz [35].
The assessment of the surface texture after the EP and other polishing processes requires the
In the classical approach, the assessment of polished surfaces based on the ARS method boiled
application of the first of the mentioned varieties of the ARS, as reported Łukianowicz [35].
down to calculating the values of the parameters defining the angular distribution of scattered light
In the classical approach, the assessment of polished surfaces based on the ARS method boiled
intensity, considered in relation to the selected plane or in space. In the first case, usually the
down to calculating the values of the parameters defining the angular distribution of scattered light
scattering angle θd was used, whose graphic form was the curve of the angular distribution of
intensity, considered in relation to the selected plane or in space. In the first case, usually the scattering
scattered light intensity. In the second case, the function was used, which was the ratio of the scattered
angle θd was used, whose graphic form was the curve of the angular distribution of scattered light
surface radiance Le (determined within the solid angle dΩ) to the incident surface irradiance. This
intensity. In the second case, the function was used, which was the ratio of the scattered surface
important function, defined in 1970 by Nikodemus [36], is known under the acronym BRDF
radiance Le (determined within the solid angle dΩ) to the incident surface irradiance. This important
(bidirectional reflectance distribution function) or BSDF (bidirectional scatter distribution function).
function, defined in 1970 by Nikodemus [36], is known under the acronym BRDF (bidirectional
Its general form is expressed by dependence (1):
reflectance distribution function) or BSDF (bidirectional scatter distribution function). Its general form
L dΦ e / dΩ 16π 2
is expressed by dependence
BRDF =(1): e = cos(θ ) cos(θ )QS ( f , f )
i d x y (1)
Φ ei / AΦ ei cosθ d λ4
where Le dΦe /dΩ 16π2
BRDF = = 4 cos(θi ) cos(θd )QS( fx , f y ) (1)
Φei /AΦei cos θd dλΦ
Le = e
(2)
Ad Ω cos θ d
Metals 2020, 10, 1098 4 of 15

where
dΦe
Le = (2)
AdΩ cos θd
and where Le —scatter surface radiance, A—illuminated surface area, dΦe —the radiant flux/power
scattered within the solid angle, dΩ—solid angle, Φei —the radiant flux/power incident of surface,
λ—wavelength of light, θi —angle of incidence, θd —scattering angle, Q—non-dimensional factor
depending on the azimuthal scattering angle φ, also allowing for the polarization state of incident light
and the optical properties of the reflecting surface, S(fx, fy)—two-dimensional surface power spectral
density function, fx, fy—spatial frequencies of the surface roughness.
With the dynamic development of modern computer programming techniques, and particularly
of new methods and algorithms of computer image processing and analysis, the assessment of the
angular distribution of scattered light intensity became possible also from its acquired digital image,
as presented by Shen et al. [37], Espinosa-Luna et al. [38], Kapłonek et al. [39], Jošt et al. [40] as well as
Kapłonek and Nadolny [41]. The image can be still, as shown by Shen et al. [37], Rao and Raj [42] as
well as Kapłonek et al. [43], or it can be also a set of moving images in the form of video sequences—this
case was discussed by Kapłonek and Łukianowicz [44]. Regardless of the form, the acquired digital
image of scattered light carries important information about the condition of the assessed surface.
This information, if properly transformed (specialized computer software) into the values of selected
geometrical and photometric parameters, can be correlated with selected surface texture parameters.
In this article, the modified ARS method supported by the image processing and analysis
techniques for assessment of surfaces after the MEP process has been presented and discussed.
Information covering the characteristics of the used samples, MEP process and acquisition of digital
images of the angular distribution of scattered light intensity is given in Section 2, whereas the obtained
experimental results with proper interpretation are presented and discussed in Section 3. At the end of
the article, a summary with the most important conclusions resulting from the experimental studies
carried out are formulated and given, as well as guidelines for future work.

2. Methodology of Experimental Studies

2.1. Characteristics of the Samples

For experimental studies, we used AISI 316L stainless austenitic steel samples, which were
prepared in the form of rectangular and square plates of dimensions 30 × 5 mm (10 samples) and
30 × 30 mm (10 samples), cut from the 1-mm metal sheet. The chemical composition of the used
material with its selected physical properties are given in Table 1.

Table 1. Chemical composition and physical properties of AISI 316L stainless austenitic steel.

Content of the Elements, wt%

Cr Ni Mo Mg Si Cu V Co C Ti P S N Fe
17.07 10.26 1.9 1.68 0.64 0.19 0.11 0.04 0.03 0.03 0.02 0.04 0.04 balance
Physical Properties
Density Hardness Specific heat Thermal conductivity (1) Melting range
7.90 g/cm3 max. 215 HB 450 J/(kg·K) (2) 14.6 W/(m·K) 1390–1440 ◦ C
Yield strength Tensile strength Elongation at break Modulus of elasticity Electrical resistivity
220 MPa 520–680 MPa 55% 193 GPa 74 µΩ·cm (3)
(1) At temperature 100 ◦ C, (2) at temperature 0–100 ◦ C, (3) at temperature 20 ◦ C.

The MEP process was performed with use of DC power supply in a magnetic field of 66 mT
and two current densities, i.e., 800 A/dm2 (MEP-800) and 50 A/dm2 (MEP-50). For the experimental
studies, a proprietary sulfuric (H2 SO4 , 95%, 98.08 g/mol)/orthophosphoric (H3 PO4 , 85%, 98 g/mol)
(40–60% by vol.) acid mixture of electrolytes without additional water was used. To eliminate any
movement in the range of 0 to 25 mm, with a positioning accuracy of 0.01 mm. As the radiation source,
a semiconductor laser, Lasiris™ SNF 635 (Coherent Inc., Santa Clara, CA, USA), which emitted a
continuous light beam from the visible spectrum range with wavelength λ = 635 nm, was used. The
beam was directed at an angle of incidence of 50° and illuminated the examined surface of the sample.
The reflected and partially scattered light from the examined surface created an optical image of
Metals 2020, 10, 1098 5 of 15
scattered light visible in the observation plane. As an observation plane, a 300 mm × 300 mm white matt
screen with scale pattern used for initial estimating of scattered light image size was used. The creation
of opticalchanges
possible images of in scattered light on
the electrolyte the observation
composition plane
due to is presented
increased in Figureno
temperatures, 2b.water was used for
For its acquisition,
the electrolyte a digital
in the study. Forcamera,
each run,Camedia C-5060WZ bycell,
the electrochemical Olympus,
made ofwhichglass,was equipped
contained with
around
a 4×cm
500 3
wide angle zoom lens 5.7–22.9 mm, was used. The camera was equipped with a matrix
of electrolyte.
photoelectric detector of CCD type, sized 1/1.8” with an effective number of 5.10 million pixels. The
2.2.
same Acquisition
acquisition of parameters
Digital Images of the
were Angular
used for allDistribution of Scattered
samples: exposure Light
time texp Intensity
= 1 s, lens stop value F4.0,
auto For
white balance, image
acquisition resolution
of digital images2592of× 1944 pixels, ISO
the angular sensitivity of
distribution 200, saving format
scattered *.jpg and
light intensity,
HQ image quality. The camera was placed on a support stand and
the experimental setup was prepared. Its general scheme is presented in Figure 2a.directed towards the observation
plane. All distances from the abovementioned elements are presented in Figure 2a.

2. Graphical scheme presenting the experimental setup used for acquisition of digital images
Figure 2.
of the angular
angular distribution
distributionof
ofscattered
scatteredlight
lightintensity:
intensity:(a)(a)
general view
general with
view keykey
with components andand
components the
the distances between them; (b) scale pattern used for initial estimating of scattered light image size;
(c) methodology of acquisition of scattered light image and main assumptions of acquisition process.

The analyzed samples were placed on an x-y stage constructed from two horizontal movement
mechanisms, type KB 11,737 (Cobrabid, Warsaw, Poland). The mechanisms provided precise sample
movement in the range of 0 to 25 mm, with a positioning accuracy of 0.01 mm. As the radiation
source, a semiconductor laser, Lasiris™ SNF 635 (Coherent Inc., Santa Clara, CA, USA), which emitted
a continuous light beam from the visible spectrum range with wavelength λ = 635 nm, was used.
The beam was directed at an angle of incidence of 50◦ and illuminated the examined surface of the
sample. The reflected and partially scattered light from the examined surface created an optical image
of scattered light visible in the observation plane. As an observation plane, a 300 mm × 300 mm
white matt screen with scale pattern used for initial estimating of scattered light image size was used.
The creation of optical images of scattered light on the observation plane is presented in Figure 2b.
For its acquisition, a digital camera, Camedia C-5060WZ by Olympus, which was equipped with a
4× wide angle zoom lens 5.7–22.9 mm, was used. The camera was equipped with a matrix photoelectric
Metals 2020, 10, 1098 6 of 15

detector of CCD type, sized 1/1.8” with an effective number of 5.10 million pixels. The same acquisition
parameters were used for all samples: exposure time texp = 1 s, lens stop value F4.0, auto white balance,
Metals 2020, 10, x FOR PEER REVIEW
image resolution 2592 × 1944 pixels, ISO sensitivity 200, saving format *.jpg and HQ image 6quality. of 15

The camera was placed on a support stand and directed towards the observation plane. All distances
distances between them; (b) scale pattern used for initial estimating of scattered light image size;
from the abovementioned elements are presented in Figure 2a.
(c) methodology of acquisition of scattered light image and main assumptions of acquisition process.
The acquisition process was realized identically for all of the examined samples. Its methodology
and mainThe assumptions are presented
acquisition process in Figure
was realized 2c. Ten
identically forpoints were
all of the designated
examined on their
samples. surface (five—
Its methodology
surface
and mainafter the MEP process,
assumptions five—base
are presented surface),
in Figure for points
2c. Ten those the
werescattered lightonimages
designated were acquired.
their surface (five—
The dimension
surface after theof MEP
measurement single point
process, five—base was 1 mm.
surface), Totalthe
for those number of acquired
scattered images
light images werefrom a single
acquired.
sample was ten.
The dimension of measurement single point was 1 mm. Total number of acquired images from a
single sample was ten.
2.3. Characteristics of Image Processing and Analysis Process
2.3. All
Characteristics
the acquired of Image Processing
digital imagesand of Analysis Process
the angular distribution of scattered light intensity were
subjected to computer analysis. Before this, the images
All the acquired digital images of the angular distribution were appropriately
of scatteredpre-processed (horizontal
light intensity were
levelling,
subjectedcropping,
to computer tonal correction)
analysis. andthis,
Before binarized in automatic
the images mode (iteration:
were appropriately 1, count:(horizontal
pre-processed 1, threshold
levels: in thecropping,
levelling, range 7.45–9.80% for MEP surface
tonal correction) and in theinrange
and binarized 15.68–19.60%
automatic for base surface).
mode (iteration: 1, count: All 1,
the
above procedures
threshold levels: were
in the carried
rangeout using ImageJ
7.45–9.80% 1.57 (W.
for MEP Rasband,
surface NIH,
and in the LOCI,
range University
15.68–19.60% of Wisconsin,
for base
surface). WI,
Madison, All the
USA).aboveThisprocedures were carried
popular Java-based imageout processing
using ImageJ and 1.57 (W. Rasband,
analysis softwareNIH,was LOCI,
widely
University ofby
characterized Wisconsin,
AbràmoffMadison, WI,
et al. [45], USA). This
Schneider popular
et al. Java-based
[46] and Rueden et image processing
al. [47]. and analysis
The prepared images
software was widely characterized by Abràmoff et al. ®
[45], Schneider et al.
were subjected to parametric analysis in Image Pro -Plus 5.1 (Media Cybernetics Inc., Rockville,[46] and Rueden et al. [47].
The USA)
MD, prepared imagesMore
software. wereinformation
subjected to parametric
about analysisprogram
this extensive in Image Pro -Plus dedicated
®
environment 5.1 (Mediato
Cybernetics
advanced image Inc., Rockville,and
processing MD, USA) was
analysis software.
given More information
by Fritzsch about
et al. [48] and this extensive
Dongming program
[49], whereas
environment dedicated to advanced image processing and analysis was
an in-depth comparison of these software programs is presented Ye et al. [50]. The methodologygiven by Fritzsch et al. [48]of
and Dongming [49], whereas an in-depth comparison of these software programs
image processing and analysis used during the experimental studies is in general form schematically is presented Ye et
al. [50]. The
presented methodology
in Figure 3. of image processing and analysis used during the experimental studies is in
general form schematically presented in Figure 3.

Figure3.3.Methodology
Figure Methodologyof of processing
processing and analysis process
process carried
carriedout
outfor
fordigital
digitalimages
imagesofofthe
theangular
angular
distribution of scattered light intensity using
distribution of scattered light intensity using ImageJ 1.57 and Pro®®-Plus 5.1 software.
and Pro -Plus 5.1 software.

Themain
The maingoal
goalofofthe
theconducted
conducted analysis
analysis was to determine
determinevalues
valuesof ofthe
thekey keyparameters
parameterswhich
which
canbebe
can useful
useful in characterizing
in characterizing these
these typestypes of images.
of images. Forpurpose,
For this this purpose, the selected
the selected functions
functions available
inavailable
Image-Pro in ®
Image-Pro Plus 5.1 software
Plus 5.1®software were used.were used.
The The function
function Count/Size,
Count/Size, an examplean example
windowwindow of
of which
which is presented on the right side in Figure 3, was realized in two steps. Step I
is presented on the right side in Figure 3, was realized in two steps. Step I involved counting all involved counting
all elements
elements in the
in the analyzed
analyzed image
image in in automaticmode,
automatic mode,giving
givingvalues
values of
of total
total counts
countsand andcounts
countsininthe
the
range.Each
range. Eachcounted
countedobject
objectin
in an
an image
image was
was labeled
labeled using
using red
redcross.
cross.In
Instep
stepII,II,the
thesoftware
softwarecalculated
calculated
thevalues
the valuesofofselected
selectedgeo-
geo-and
and photometric
photometric parameters
parameters (from
(frommore
morethan
than50 50available)
available)with
withstatistical
statistical
summary. An example window of the Statistics function is presented on the right side in Figure 3. This
summary included selected statistical values (minimum (min.), maximum (max.), average (mean),
standard deviation (std. dev.) and accumulated (sum)) calculated for the declared parameters.
In general, interesting parameters which may be relevant in the analysis of images of the angular
distribution of scattered light intensity are those representing geo- and photometric groups. Since the
Metals 2020, 10, 1098 7 of 15

summary. An example window of the Statistics function is presented on the right side in Figure 3.
This summary included selected statistical values (minimum (min.), maximum (max.), average (mean),
standard deviation (std. dev.) and accumulated (sum)) calculated for the declared parameters.
In general, interesting parameters which may be relevant in the analysis of images of the angular
distribution of scattered light intensity are those representing geo- and photometric groups. Since the
authors used the Image-Pro® Plus environment, they chose one key parameter each from the groups
available in this software. As a key geometric parameter, the area (of the bright regions of an image of
scattered light) An was proposed. The values of An can be calculated from dependence (3), given below:

N−1
X N−1
X
An = I (i, j) (3)
i=0 j=0

where i, j—coordinates of the corresponding image elements (i—row number, j—column number),
I(i, j)—grey scale intensity.
From the group of photometric parameters, the integrated optical density (of the bright regions
of an image of scattered light) I Σ was proposed. In this case, values of I Σ can be calculated from
dependence (4), given below: X
IP = I (i, j) (4)
i,j∈An

where i, j—coordinates of the corresponding image elements (i—row number, j—column number),
I(i, j)—grey scale intensity, An—image area.
The values of the above parameters were obtained using the Count/Size function, whereby for An,
the values were calculated for images after binarization (all the dark objects were counted), and for IΣ
from input images without binarization (all the bright objects were counted).

3. Results and Discussion

In this section, selected results of acquisition and analysis of images of the angular distribution
of scattered light intensity are presented and discussed. The acquisition process realized using the
experimental setup (described in Section 2.2) allowed us to obtain a set of scattered light images.
Examples of images acquired for two different types of samples (MEP-800 and MEP-50) are presented
in Figure 4.
The polished surface after the MEP process is characterized by relatively high anisotropy.
This means that, regardless of the direction of incidence of the laser beam, the angular distribution of
the scattered light intensity should take the same form. Typically, the distribution of the scattered light
intensity of such a surface is situated on a straight line segment, being the intersection of the incidence
plane and observation plane. The resulting image is thus close to a point and takes the form of a circle
(Figure 4a) or an ellipse (Figure 4b). In some cases, the above forms can be visually supplemented with
additional angular distribution(s) of scattered light intensity resulting from the occurrence of various
types of defects on the analyzed surface. These defects, defined by the EN-ISO 8785:1999 standard [51]
and appearing under the acronym SIM (surface imperfections), in this case occurred on both surfaces
shown in Figure 4 in the form of scratches.
Metals 2020, 10, 1098 8 of 15

Metals 2020, 10, x FOR PEER REVIEW 8 of 15

Figure4.4. Collection
Figure Collection of
of example
example results
results of
ofacquisition
acquisition of
ofdigital
digitalimages
imagesofofthe
theangular
angulardistribution
distributionof
of
scatteredlight
scattered lightintensity
intensitycarried
carriedout
outfor
forsurface
surfaceafter
afterthe
theMEP
MEPprocess,
process,transition
transitionlayer
layerand
andbase
basesurface
surface
occurringon
occurring onsample:
sample: (a)
(a) MEP-800;
MEP-800; (b)
(b)MEP-50.
MEP-50.

The
Theresults
resultsofofimage
imageanalysis
analysisin inthe
theform
formofofthe
the calculated
calculatedvalues
valuesof ofthe
the area
area(of(of the
the bright
bright regions
regions
of
of scattered light image) and integrated optical density (of the bright regions of scattered light image)
scattered light image) and integrated optical density (of the bright regions of scattered light image)
parameters
parametersare arepresented
presentedin inFigures
Figures55andand6,6,respectively.
respectively.
In Figure
In Figure 5a,b, 5a,b, bar graphs
bar graphs presenting
presenting calculated
calculated values values of the
of the area (ofarea (of theregions
the bright bright of regions of
scattered
scattered light image) for all analyzed MEP-800 and MEP-50 samples are shown.
light image) for all analyzed MEP-800 and MEP-50 samples are shown. The light gray bar is a valueThe light gray bar is
acalculated
value calculated for the surface
for the surface after theafter
MEP, the MEP, whereas
whereas the darkthe dark
gray bargray bar is calculated
is a value a value calculated for
for the base
the base The
surface. surface. The red
red dotted dotted
line line represents
represents an averageanvalue.
average value.
These valuesThese values
obtained forobtained
both typesfor of
both
the
samples were at the same level. For the MEP-800 samples (Figure 5a), the following mean values
were obtained: Anavr = 603.965 mm2, min. Anavr = 551.596 mm2 (MEP-800-7) and max. Anavr = 551.596
mm2 (MEP-800-6). Meanwhile, for the MEP-50 samples (Figure 5b), the following mean values were
Metals 2020, 10, 1098 9 of 15

types of the samples were at the same level. For the MEP-800 samples (Figure 5a), the following
mean values were obtained: Anavr = 603.965 mm2 , min. Anavr = 551.596 mm2 (MEP-800-7) and max.
An avr =
Metals
551.596 mm2 (MEP-800-6). Meanwhile, for the MEP-50 samples (Figure 5b), the following
2020, 10, x FOR PEER REVIEW 9 of 15
mean values were obtained: Anavr = 664.191 mm2 , min. Anavr = 514.952 mm2 (MEP-50-6) and max.
avr = 811.716
An 2 (MEP-50-2).
obtained: Anavr =mm 664.191 mm2, min.The Anavrsurface after
= 514.952 mm the MEP was characterized
2 (MEP-50-6) and max. Anavrby 49% (MEP-800)
= 811.716 mm2 (MEP- and
over
50-2).49%The(MEP-50)
surface after theAn
lower MEP values than the baseby
was characterized surface. Additionally,
49% (MEP-800) and overthe MEP surface showed
49% (MEP-50) lower
much better reflection
An values than the properties
base surface. thanAdditionally,
the base surface.the The
MEPcreatedsurfaceimage
showed of themuch
angular distribution
better reflectionof
scattered
properties light
thanintensity
the base was close toThe
surface. a circle—typical
created image forofpolished surfaces
the angular with smallofheights
distribution of surface
scattered light
irregularities.
intensity wasA close similartosituation was observed
a circle—typical for for values of
polished the photometric
surfaces with small parameter
heights ofofintegrated
surface
optical densityA(of
irregularities. the bright
similar regions
situation was of scattered
observed forlight
values image),
of thepresented
photometric in parameter
Figure 6a,b, ofrespectively.
integrated
optical
For density (of
the MEP-800 the bright
samples regions
(Figure of scattered
6a), the followinglight
mean image),
valuespresented
were obtained:in Figure = 363,442.542
IΣavr6a,b, respectively.
a.u.,
For the
min. = 324,545.131
IΣavrMEP-800 samples a.u.(Figure 6a), theand
(MEP-800-2) following
max. IΣavrmean = 463,945.195
values werea.u. obtained: IΣavr = 363,442.542
(MEP-800-6). Meanwhile,
a.u.,
for themin. IΣavr = samples
MEP-50 324,545.131 a.u. (MEP-800-2)
(Figure and max.
6b), the following mean IΣavrvalues
= 463,945.195 IΣavr = 388,694.281
a.u. (MEP-800-6).
were obtained: Meanwhile, a.u.,
for the
min. IΣavr = 302,339.5
MEP-50 samples (Figure
a.u. 6b), theand
(MEP-50-6) following mean
max. IΣavr = 500,471.31
values were obtained:
a.u. IΣavr = 388,694.281
(MEP-50-2). The surfacea.u.,
after
min.
the MEP IΣavrwas
= 302,339.5 a.u. (MEP-50-6)
characterized and max.and
by 51% (MEP-800) IΣavr54%
= 500,471.31
(MEP-50)a.u. (MEP-50-2).
lower I Σ valuesThethansurface
the baseafter the
surface.
MEP was characterized by 51% (MEP-800) and 54% (MEP-50) lower I
These values confirmed the earlier trend of An values and also closely corresponded to the visually Σ values than the base surface.
These values
analyzed images confirmed the earlier
of the angular trend of An
distribution values and
of scattered also
light closely corresponded to the visually
intensity.
analyzed images of the angular distribution of scattered light intensity.

Figure 5. Average values of area (of the bright regions of scattered light image) obtained for surface
Figure 5. Average values of area (of the bright regions of scattered light image) obtained for surface
after the MEP process and base surface for samples (a) MEP-800; (b) MEP-50.
after the MEP process and base surface for samples (a) MEP-800; (b) MEP-50.
Metals 2020, 10, 1098 10 of 15
Metals 2020, 10, x FOR PEER REVIEW 10 of 15

Figure6.6.Average
Figure Averagevalues
values ofof integrated
integrated optical
optical density
density (of
(ofthe
thebright
brightregions
regionsofofscattered
scatteredlight
lightimage)
image)
obtainedfor
obtained forsurface
surfaceafter
afterthe
theMEPMEPprocess
process and
and base
base surface for samples
samples (a)
(a)MEP-800;
MEP-800;(b) (b)MEP-50.
MEP-50.

For
Forthe
theconducted
conductedcomparative
comparative analysis
analysis of the obtained
obtained results,
results,aasetting
settingofofthe
thevalues
valuesobtained
obtained
duringthe
during the previously
previously conducted
conductedexperimental
experimental studies
studieswas prepared.
was To facilitate
prepared. comparison,
To facilitate two
comparison,
surfaces made of AISI 316L stainless austenitic steel after the electrochemical polishing
two surfaces made of AISI 316L stainless austenitic steel after the electrochemical polishing (EP, MEP), (EP, MEP), as
aswell
wellasasfour
foursurfaces
surfacesmade
madeofofgray
graycast
castiron
ironGJL
GJL150,
150,brass
brassCWCW612N,
612N,aluminum
aluminum alloy AW-6082
alloy AW-6082and and
carbonsteel
carbon steelC45
C45after
afterthe
theconventional
conventional machine
machine polishing
polishing (CMP;
(CMP;realized
realizedbybyusing
usingabrasive
abrasivesheets
sheets
andAlAl
and 2O3-based polishing paste), were selected. For all the samples compared, digital images of the
2 O3 -based polishing paste), were selected. For all the samples compared, digital images of the
angular distributionof
angular distribution ofscattered
scatteredlight
light intensity
intensity were
were acquired
acquired and
andthe
theaverage
averagevalues
valuesofofareas
areas(of
(ofthe
the
brightregions
bright regionsofofscattered
scatteredlight
lightimage)
image)were were calculated.
calculated. These
These values
values were
were correlated
correlatedwithwiththe
thebasic
basic
roughness(profile)
roughness (profile)parameter—the
parameter—the roughness
roughness average
average Ra.
Ra. The
Theused
usedexperimental
experimentalsetupsetupallowed
allowedusustoto
measure this in a range from ~0.02 to ~1 µm. Additionally, the Ra values were measured alsoby
measure this in a range from ~0.02 to ~1 μm. Additionally, the Ra values were measured also byusing
using
an optical profilometer Talysurf CLI 2000 (Taylor-Hobson, Leicester, Great Britain) equipped witha a
an optical profilometer Talysurf CLI 2000 (Taylor-Hobson, Leicester, Great Britain) equipped with
lasertriangulation
laser triangulationsensor
sensorLK-031
LK-031 (Keyence
(Keyence Corp.,
Corp., Osaka,
Osaka, Japan).
Japan). This
Thisconfiguration
configurationallowed
allowedusustoto
conduct surface roughness measurements in a range up to 10 mm at resolutions of 1 μm (vertical)
conduct surface roughness measurements in a range up to 10 mm at resolutions of 1 µm (vertical) and
and 30 μm (lateral). A detailed description of the measurement capabilities and selected application
30 µm (lateral). A detailed description of the measurement capabilities and selected application of
of this measurement system are given by Kapłonek et al. [52]. The correlation between the geometrical
this measurement system are given by Kapłonek et al. [52]. The correlation between the geometrical
parameter calculated from the image An and profile parameter Ra is presented in Figure 7.
parameter calculated from the image An and profile parameter Ra is presented in Figure 7.
Metals 2020, 10, 1098 11 of 15
Metals 2020, 10, x FOR PEER REVIEW 11 of 15

Figure
Figure 7. 7.
TheTheset
setofofaverage
average values
valuesofofAn Anarea (of(of
area thethe
bright regions
bright of scattered
regions light image)
of scattered vs. Ra vs.
light image)
roughness average
Ra roughness averagefor forsurfaces
surfacesafter finishing
after by various
finishing variations
by various of theofpolishing
variations process.
the polishing process.

TheThe values
values presented
presented in Figure
in Figure 7 allow
7 allow usstate
us to to state
that that the MEP
the MEP process
process is over
is over 32% 32%
moremore
effective
thaneffective
EP. Thethan EP. The
obtained obtained
surface hassurface has lower
over 27% over 27% lower roughness
roughness and much and muchreflection
better better reflection
properties,
properties, making it more advantageous. Comparison of surfaces after electrochemical polishing
making it more advantageous. Comparison of surfaces after electrochemical polishing (EM, MEP) and
(EM, MEP) and conventional machine polishing (CMP) shows that CMP is over 68% more effective.
conventional machine polishing (CMP) shows that CMP is over 68% more effective. The values of the
The values of the Ra parameter decrease significantly, which indicates a relatively smooth surface
Ra parameter decrease significantly, which indicates a relatively smooth surface with small heights of
with small heights of the surface irregularities (from Ra = 0.036 to 0.069 μm). High surface smoothing
the positively
surface irregularities
affects the reflection = 0.036 towhich
(from Raproperties, 0.069isµm). High for
important surface
thesesmoothing positively affects the
types of surfaces.
reflection properties, which is important for these types of surfaces.
4. Conclusions
4. Conclusions
In the preliminary experimental studies presented in this article, the authors showed that one of
In proposed
the the preliminary experimental
light-scattering studies presented in
methods—angle-resolved this article, the
scattering—can be authors showed
successfully usedthat
for one
of the
assessment of surfaces after electrochemical polishing in a magnetic field in relation to geo- and for
proposed light-scattering methods—angle-resolved scattering—can be successfully used
assessment
photometricof surfaces
parameters. after electrochemical
Below, polishing
the most important in a magnetic
conclusions fieldfrom
resulting in relation
the researchto geo-
are and
given.
photometric parameters. Below, the most important conclusions resulting from the research are given.
1. The AISI 316L stainless austenitic steel samples divided into two groups (each 10 samples) were
1. Theelectrochemically
AISI 316L stainless austenitic
polished steelfield:
in a magnetic samples
MEP-800divided into field:
(magnetic two groups (each 10
66 mT, current samples)
density:
were800electrochemically
A/dm2) and MEP-50 polished
(magneticin field:
a magnetic
66 mT, field:
current MEP-800 (magnetic
density: 500 A/dm2) field:
(Section 66 2.1).
mT, The
current
density:
samples800after
A/dm the2 )process
and MEP-50 (magnetic field:
were characterized 66 mT, current
by relatively smoothdensity: small2heights
500 A/dm
surface with ) (Section
of 2.1).
the surface irregularities. The average value of Ra roughness (profile)
The samples after the process were characterized by relatively smooth surface with small parameter measured by
opticalof profilometer
heights Talysurf CLI 2000
the surface irregularities. with laser
The average triangulation
value of Ra roughnesssensor (profile)
LK-031 for all
parameter
magnetoelectropolished
measured by optical profilometersurfaces Talysurf
was 0.823CLI μm.2000 with laser triangulation sensor LK-031 for all
2.magnetoelectropolished
The obtained surface features were assessed
surfaces was 0.823 µm. by using one of the non-contact light-scattering
methods for confirmation of correctness of carrying out the process. In this case, the angle-
2. The obtained surface features were assessed by using one of the non-contact light-scattering
resolved scattering-based experimental setup was used. The surface of each sample was
methods for confirmation of correctness of carrying out the process. In this case, the angle-resolved
illuminated using a laser beam (wavelength λ = 635 nm, angle of incidence 50°) and its angular
scattering-based
distribution in experimental
the observation setup was
plane wasused. The surface
acquired of each
as a digital sample
image was2.2).
(Section illuminated
After pre- using
a laser beam (wavelength
processing λ = 635we
(ImageJ 1.57) images, nm, angleout
carried of parametric ◦
incidence analysis
50 ) and(Image
its angular distribution
Pro®-Plus 5.1), which in the
observation
included the plane was acquired
calculation of twoas keya digital
geo- and image (Sectionparameters
photometric 2.2). After(Section
pre-processing
2.3). (ImageJ 1.57)
3.images, we carried
The obtained valuesoutofparametric analysis
area (of the bright (Image
regions Pro® -Plus
of scattered light5.1), which
image) included
(Figure 5) andthe calculation
integrated
optical density (of the bright regions of
of two key geo- and photometric parameters (Section 2.3).scattered light image) (Figure 6) were similar for the
3. Themagnetoelectropolished
obtained values of area surfaces
(ofofthe
both types regions
bright of samples.of Additionally,
scattered light we found
image) that the above
(Figure 5) and
values (in each case) were approx. 50% lower (An MEP—49% (MEP-800) and over 49% (MEP-50);
integrated optical density (of the bright regions of scattered light image) (Figure 6) were similar
IΣMEP—51% (MEP-800) and 54% (MEP-50), respectively) than those obtained for the base surface.
for the magnetoelectropolished surfaces of both types of samples. Additionally, we found that
the above values (in each case) were approx. 50% lower (AnMEP —49% (MEP-800) and over 49%
(MEP-50); IΣMEP —51% (MEP-800) and 54% (MEP-50), respectively) than those obtained for the
Metals 2020, 10, 1098 12 of 15

base surface. This indicates a much smaller share of light scattering component at the gain
of the specular reflection component. This is a very advantageous surface feature after the
magnetoelectropolished process, especially useful in a wide range of industrial applications,
in areas such as precision mechanical, chemical and biomedical engineering as well as opto-
and microelectronics.
4. Compared to electropolishing, the magnetoelectropolishing process is characterized by over 32%
more effectiveness (Figure 7) at 27% lower surface roughness (Ra). The results obtained for this
type of surface (in the context of their reflection properties and surface texture properties) are very
promising, which encourages further work to improve this electrochemical polishing process and
study its effects.

Author Contributions: Supervision, W.K.; conceptualization, W.K., K.R., D.Y.P., research methodology, W.K., K.R.,
D.Y.P., investigation, W.K., K.R.; formal analysis, D.Y.P.; writing—original draft preparation, W.K.; writing—review
and editing, K.R., D.Y.P. All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Conflicts of Interest: The authors declare no conflict of interest.

Nomenclature
AC Alternating current
AFM Atomic force microscopy
ARS Angle-resolved scattering
BRDF Bidirectional reflectance distribution function
BSDF Bidirectional scatter distribution function
CCD Charge-coupled device
CLSM Confocal laser scanning microscopy
CMP Conventional machine polishing
DC Direct current
EP Electropolishing
FVM Focus variation microscopy
MEP Magnetoelectropolishing
MFM Mirror facet model
PSI Phase shifting interferometry
SIM Surface imperfections
SEM Scanning electron microscopy
T-S Torrence–Sparrow theory
A Illuminated surface area
An Area (of the bright regions of an image of scattered light)
dΦe Radiant flux/power scattered within the solid angle
dΩ Solid angle
An Area (of the bright regions of an image of scattered light)
fx Spatial frequency (x-axis) of the surface roughness
fy Spatial frequency (y-axis) of the surface roughness
I(i, j) Grey scale intensity
IΣ Integrated optical density (of the bright regions of an image of scattered light)
i Row number
j Column number
Le Scatter surface radiance
Q Non-dimensional factor depending on the azimuthal scattering angle φ
Ra Roughness average
S(fx, fy) Two-dimensional surface power spectral density function
θi Angle of incidence
θd Scattering angle
λ Wavelength of light
Φei Radiant flux/power incident of surface
Metals 2020, 10, 1098 13 of 15

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