©2017 International Transaction Journal of Engineering, Management, & Applied Sciences & Technologies.

International Transaction Journal of Engineering,

Management, & Applied Sciences & Technologies
[Link]

Improvement of Electrolytic Etching on Stainless Steel

Grade SUS 304
a* a b
Apiwat Muttamara , Natta Naulpring and Somsak Siwadamrongpong
a
Department of Industrial Engineering, Faculty of Engineering, Thammasat University, Pathumtani,
THAILAND
b
Manufacturing Engineering, Faculty of Engineering, Suranaree University of Technology, Nakhon
Ratchasima, THAILAND.
ARTICLEINFO ABSTRACT
Article history: The objective of this study is to improve production rate for bio-medical
Received 28 February
2017 devices stainless tube. In particular, attention is focused on parameters of the
electro-etching procedure into the manufacturing process for stainless wire.
Received in revised form
12 June 2017 The wire is used for angiography or arteriography that is a medical imaging
Accepted 16 June 2017
Available online technique used to visualize the inside, or lumen, of blood vessels and organs
19 June 2017 of the body, with particular interest in the arteries, veins, and the heart
Keywords: chambers, so quality of work is important. Electrolytic etching is technique
Scanning electron which gives fine, bright and stress-free surface. This paper reports the
microscopy; material findings of an experimental investigation on Electrolytic etching of SUS304
removal rate; stainless steel. In this investigation, effect of process parameters on
electrolyte lifetime; performance measure as diameter reduction rate was studied. The process
etching process; parameters which were chosen were: current (A) and electrolysis time (min.).
bio-medical devices;
The relation between current and material removal was proposed. The results
electrolysis time;
stainless tube;
and the significance of controlling parameters were analyzed using analysis of
arteriography; variance (ANOVA). It was found that current is a significant parameter. The
workpiece; ANOVA. electrolysis time and the number of workpiece for each lot sizes were
investigated.

© 2017 INT TRANS J ENG MANAG SCI TECH.

1. Introduction
In the biomedical field, quality of work is important. Electrolytic etching is especially useful
for the finish machining of stainless steel wire. The wire is used for angiography or arteriography
with particular interest in the arteries, veins, and the heart chambers. Electrolytic etching does not
induce surface stress, promoting the preferential removal of surface roughness [1,2]. The
dissolution rate of the metallic surface is significantly increased by the application of anodic
currents [3,4]. Electrolytic etching is normally performed in an appropriate solution under suitable
*Corresponding author (A. Muttamara).. E-mail: mapiwat@[Link]. ©2017. International
Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. Volume 8 49
No.1 ISSN 2228-9860 eISSN 1906-9642. Online Available at [Link]
conditions [4]. There are many factors that affect to the quality of the finished product. Life time of
dissolute is involved to environment. The more use of dissolute may be extended. Such factors
include current density, concentration and temperature of solution, polishing duration, frequency of
applied current, and the method of agitation [5- 7]. The process consists of an anode (work piece),
a cathode (electrode) and electrolyte. Generally, the electrolyte is composed of viscous acid fluid.
During the anodic dissolution, the dissolution rate at the anode is the slowest and is the controlling
factor [8]. Therefore, the electrochemical reaction is under diffusive mechanism. Due to the
diffusive mechanism, a viscous film will be formed on the anode. The increase in resistance of the
viscous film prevents the electrochemical reaction efficiency from increasing [6]. The surface is
basic-ally etched in an acid bath and in parallel an electric field is applied to the surface which in
turns causes a current flow. Because of the current enhancement, sharp tips on the surface are
removed. For most metals one finds similar current density-voltage curve for the electrochemical
polishing process [7]. The detailed shape of the curve depends on the ratio of surface area of
cathode and anode and the initial surface roughness [9]. During electrolyte etching, positive metal
ions leave the specimen surface and diffuse into the electrolyte, an equivalent number of electrons
remains in the materials.

2. Experiment procedure
Specimens of SUS–304 stainless steel rod of size 120 mm length and 0.05 mm diameter were
cut and their sharp edges and burrs were remove on grinder as shown in Figure 1. As the specimens
have rolling marks, surface defects scratches and scales, initial mechanical polishing is needed.
After mechanical polishing, specimens were clean in running tap water, dried and solvent
degreased. It is then weighed. Before polishing, specimen is dipped in hot steelex 20 (alkaline soap
cleaner) solution for 5-10 minutes. Its temperature was maintained approximately 70-800°C.

Figure 1: Experimental setup of etching process and finish product.

After soaking, steel specimen maintains approximately 70-800°C. After soaking, steel
specimen cleaned in running water then dipped in 10% HCL for 10-20 seconds to remove alkaline
film formed on the specimen. It is then cleaned in running water followed by cleaning in distilled.
Evenly spread thin film of distilled water on specimen indicates that specimen is completely clean.
Then specimen is dried and stored on clean paper. And then, specimens were immersed in

50 Apiwat Muttamara, Natta Naulpring and Somsak Siwadamrongpong

electrolyte (500ml H2 SO4 + 340ml H3PO4 + 100ml HOC-COOH + 3.5gm/100ml K2 CR2O7 + 60ml
distilled water per liter). The diameter of finished product is 0.028 – 0.034 millimeter. For
parameters was set up on Table 1. Voltage is fixed at 18 volts. It has been reported that the voltage
for electro-polishing affect to surface’s quality [10]. The influence of temperature, applied current
and time on surface roughness reduction were investigated by the analysis of variance (ANOVA)
and the obtained results were followed by scanning electron microscopy measurements.

Table 1: Experimental conditions

Parameters Value
Electrode SUS304
Workpiece SUS304
Workpiece height 120 mm
Etching area ( Ø 0.05 x 37 mm) 5.81 mm2
Current density 0.2 – 0.4 A
Number of workpiece / etching 4 pcs

3. Results and Discussions

For electrolytic etching, current density is a function of the process. The current density is a
function of the ohm resistance. Figure 2 shows relationship between current and material removal
rate (MRR). The highest MRR value occurs at the highest current density. However, if the current is
set more than 0.4 ampres the surface of workpiece was burned. Moreover, increasing the current
density makes result in a smoother and more polished surface while more material loss, due to an
increase in the mass transport rate [10 ].
0.0009
0.0008
Material Removal Rate

0.0007
(mm3/ min.)

0.0006
0.0005
0.0004
0.0003
0.0002
0.0001
0
0 0.1 0.2 0.3 0.4 0.5
Current (A)

Figure 2: Relationship between current and material removal rate (MRR).

ANOVA (Analysis of Variance) is a statistical tool for obtaining the contribution of variable
parameters. The purpose of the analysis of variance (ANOVA) is to reveal the process parameters
that significantly affect the performance characteristics. Using the experimental design module in
the MINITAB, one obtains the results as shown in Table 2. A statistical tool called a P value can be
used to identify the factors that significantly affected on the quality characteristic. In performing the
P value is less than 0.05. In this study by using ANOVA the contribution of current shows its
interaction towards MRR. In the table DF is for degree of freedom, SS for sum of squares, MS for
*Corresponding author (A. Muttamara).. E-mail: mapiwat@[Link]. ©2017. International
Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. Volume 8 51
No.1 ISSN 2228-9860 eISSN 1906-9642. Online Available at [Link]
mean of square and F value is the ratio of regressions mean square and mean square error. The
standard deviation of errors in the modelling (s=0.0005774) indicates that the model is capable of
predicting the response with a high response.

Table 2: Results of ANOVA.

Source DF SS MS F P
Current 3 0.003091 0.0010303 3091 0.000
Error 8 0.0000027 0.0000003
Total 11 0.0030937
S = 0.0005774 R-Sq = 99.91% R-Sq(adj) = 99.88%

The influence of electrolyte concentration on the precision process is highlighted using

empirically adjusted formulae. In Industrial practice optimum concentration is found by trial and
error to give the desired specification. The solution should have ion concentration. Electrode
reaction kinetics are affected by the electrode surface cleanliness, surface microstructure, and
surface chemistry.

The quality of the surface obtained by electrochemical polishing strongly depends on the
electrolyte properties[1-2]. However, appropriate use affect to health hazards and environmental.
Irritation, corrosive injuries and burns have a direct impact on the workers in the field. Improper
disposal of chemical etchants changes the level of acidity and alkalinity affect the flora and fauna in
soil and water. Normally, electrolyte can be used for 46 times (each time sets for 4 pieces). It means
that 184 of workpieces were used for etching. The test was carried out to investigate reused
electrolyte. The second lot was carried out with the same electrolyte. Figure 3 shows relationship
between etching time to diameter of workpiece with first electrolyte and second electrolyte using
current 0.4 Amperes.

Figure 3: Relationship between etching time to diameter of workpiece with first electrolyte and
second electrolyte.

The workpiece can thus be predicted and controlled to improve the dimensional accuracy of the
process. The result shows that first electrolyte can control the specification of 0.028–0.034 mm.
From the results, etching time = 66 seconds make workpiece lower specification. So, suitable

52 Apiwat Muttamara, Natta Naulpring and Somsak Siwadamrongpong

values of processing time are 56-62 seconds. From Figure 3(b), when the test were carried out in
second electrolyte. The processing time was used longer than that of new electrolyte. Lifetime of
electrolyte was reduced with ion concentration of the etching liquid. The new electrolyte enables
higher accuracy to be realised than with lower ion concentration electrolyte. For second electrolyte,
etching time can be used during 57–61 seconds. Figure 4 shows SEM of finished surface after the
process compared with first electrolyte and second electrolyte. Figure 4(b) displays the etched
surface of specimen with second electrolyte. The result show that etched surface after second
electrolyte is rougher than that of finished surface with first electrolyte. When a process is stably
done and in control, it displays common cause variation, which is inherent to the process. A
process is in control when based on past experience it can be predicted how the process will vary
within limits. When a process operates in this condition, that process is in control and produces 100
percent conformance [11].

a) First electrolyte b) Second electrolyte

Figure 4: SEM of finished surface after the process with

a) First electrolyte and b) Second electrolyte

Relatively surface roughness resulted normal electrolyte and used electrolyte are shown in SEM
Figure 4. The craters on surface etched in used electrolyte (Figure 4b) are larger than the craters on
that etched in new electrolyte (Figure 4a). The surface roughness is declined with diluted
electrolyte concentration. This is because the higher electrolyte concentrations make the stronger
activation. Then, the oxide film will have very little effect on ECM as the concentration increases.
The dissolution of the elements in the alloy will be uniform, and the surface roughness is better.
The present study deals with the objective of finding process parameters to yield the machining
time by the design of experiment. The quality of the surface obtained by electrochemical polishing
strongly depends on the electrolyte properties. Appropriate care has to be taken when using this
solution due to environmental and health hazards. Number of workpiece can be used with 370
pieces. It is possible that more workpieces may accept, due to quality of surface obtained within
specifications.

*Corresponding author (A. Muttamara).. E-mail: mapiwat@[Link]. ©2017. International

Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. Volume 8 53
No.1 ISSN 2228-9860 eISSN 1906-9642. Online Available at [Link]
 Table 4: Analysis of Variance for S/N ratios for MRR
Source DF SS MS F P
Concentration 2 0.0000021 0.0000011 1.78 0.183
Etching time 5 0.0002429 0.0000486 81.98 0.000
Interaction 10 0.000003 0.0000003 0.51 0.874
Error 36 0.0000213 0.0000006
Total 53 0.0002693
S = 0.0007698 R-Sq = 92.08% R-Sq(adj) = 88.34%

The Two-Way ANOVA was used for analyze of the parameters (electrolysis time and
concentration of electrolysis). The table showed the P-value under 0.05 in case of electrolysis time
but P-value of validated electrolysis is over 0.05. It is comprehended that electrolysis time is
noticeable significant factor. However, electrolytic concentration is not significant. The total sum
of the squared deviations was decomposed into two sources as sum of the squared deviations due to
each process parameters. The percentage of contribution of each process parameter in the total sum
of the squared deviations can be used to evaluate the importance of each process parameters over
the performance characteristic. The F value test was also used to investigate the degree of
significance of each process parameter over the performance. Usually, the largest value of F
recorded the most significant process parameter.

4. Conclusions
The paper presented improvement of Electrolytic Etching on Stainless Steel Grade SUS 304 by
experiment. As a result, the target performance characteristics can be concluded.
• The quality of the surface obtained by electrochemical polishing strongly depends on
currents and the etching time that is verified by experiment and analysis of variance.
• The quality of the workpiece that are included precision dimension and surface roughness,
preliminarily assessed by visual inspection, could be confirmed by scanning electron
microscopy.
• Processing time is 56-62 seconds for normal electrolyte.
• Processing time is during 57 – 61 seconds for the second electrolyte.

5. Acknowledgements
The authors gratefully acknowledge the financial support provided by Thammasat University
Research Fund under TU Innovative Scholar and the National Research University Project of
Thailand Office of Higher Education Commission. The authors are grateful to Asahi Intecc
(Thailand) Co.,Ltd for all the facilities made available.

6. References
[1] W.J. McG Tegart, “The Electrolytic and Chemical Polishing of Metals,” 2nd ed., Pergamon
Press, London, 1959.
[2] D.R. Gabe, L.L. Sheir, R.A. Jarman, and G.T. Burstein (Eds.), “Corrosion, volume.2,
Butterworths-Heinemann, Oxford, 1994, p.11-39.

54 Apiwat Muttamara, Natta Naulpring and Somsak Siwadamrongpong

[3] K.P. Rajurkar, C.L. Schnacker, “Some aspects of ECM performance and control,” CIRP 37 (1),
1988. p. 183–186.
[4] H. Zhao, J. Van Humbeeck, and I. De Scheerder, “Surface conditioning of nickel-titanium alloy
stents for improving biocompatibility,” Surface Engineering, 17 (6), 2001, p. 451- 458.
[5] C. L. Faust, “Surface Preparation by Electropolishing”, Journal of the Electrochemical Society,
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[6] E. S. Lee, “Machining Characteristics of the Electropolishing of Stainless Steel (STS316L)”,
The International Journal of Advance Manufacturing Technology, Vol. 16, 2000, p. 591-
599.
[7] G. R. Kamat, “Pitting and its Control During Electropolishing of Stainless Steel”, Transactions
of the Indian Institute of Metals, Vol. 40, no.4, 1987, p. 343-345.
[8] [Link], T.Z. Quazi and V.J. Pillewan, The Effect of Electrochemical Polishing on Diameter
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Research In Science & Engineering (IJAFRSE), Vol. 1, Special Issue , Vivruti 2015, p. 1-7.
[9] H. El-Hofy and H. Youssef, Environmental Hazards of Nontraditional Machining Proceedings
of the 4th IASME / WSEAS International Conference on ENERGY & ENVIRONMENT
(EE'09), p.140-145.
[10] Anshuman Bhuyan, Brandon Gregory, Howard Lei, Seow Yuen Yee, Yogesh B.
Gianchandani, Pulse and DC Electropolishing of Stainless Steel for Stents and Other
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[11] A.K.M. De Silva, H.S.J. Altena, J.A., Influence of Electrolyte Concentration on Copying
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[Link] Muttamara is an Assistant Professor of Department of Industrial Engineering at Thammasat University.

He received his [Link]. from Kasetsart University and the [Link]. in Materials Science from Nagaoka University of
Technology, Japan. Dr. Muttamara is interested involve Electrical Discharge Machining of insulating materials.

Natta Naulpring obtained her Master of Engineering degree in Industrial Work Development from Thammasat
University. Her research focuses on efficiency improvement of electrolytic etching on stainless steel.

[Link] Siwadamrongpong is teaching in Manufacturing Engineering, Faculty of Engineering, Suranaree

University of Technology, Nakhon Ratchasima, Thailand. He obtained his [Link]. (Mechanical Engineering) from
Chulalongkorn University, Thailand. He got his master degree in Environmental System Engineering from Nagaoka
University of Technology, Japan, and his PhD in Energy and Environment Science also from Nagaoka University of
Technology, Japan. [Link] research encompasses Material Characteristics, Reliability of Product,
Processes and Parts, and Jig & Fixture Design for Manufacturing / Maintenance.

*Corresponding author (A. Muttamara).. E-mail: mapiwat@[Link]. ©2017. International

Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. Volume 8 55
No.1 ISSN 2228-9860 eISSN 1906-9642. Online Available at [Link]