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Procedia CIRP 42 (2016) 412 – 417

18th CIRP Conference on Electro Physical and Chemical Machining (ISEM XVIII)

Selection and Optimization of Electrolyte for Micro Electrochemical

Machining on Stainless Steel 304
Liu Guodong a, Li Yong a*, Kong Quancun a,b, Tong Hao a
a
Department of Mechanical Engineering, Beijing Key Lab of Precision / Ultra-precision Manufacturing Equipments and Control, Tsinghua University, Beijing
100084, China;
b
School of Instrumentation Science and Opto-Electronics Engineering, Beijing Information Science & Technology University, Beijing 100192, China
* Corresponding author. Tel.: +86-010-62772212; fax: +86-010-62796339. E-mail address: liyong@mail.tsinghua.edu.cn

Abstract

During the process of micro electrochemical machining (Micro ECM) of metallic alloys, insoluble electrolytic products restrict the depth of
micro holes with high aspect ratio. The selection and optimization of composite electrolyte are researched to dissolve and remove electrolytic
products smoothly. Composite electrolyte containing neutral salt and complexing agents is adopted, in which the ligands are utilized to generate
soluble products with metal ions. To optimize the electrolyte constituent, products deposition on electrode surface, inlet diameter, material
removal rate (MRR) and ratio of removal rate to current (MRC) are taken as evaluation criterions. Micro ECM experiments on stainless steel
304 (SS304) are carried out. The electrolyte which contains 1.0 mol/L NaNO3 and 0.01 mol/L sodium citrate is selected as optimal constituent.
Micro holes with diameter of 160~190 μm are achieved on SS304 with 0.5 mm thickness. Experimental results show that the MRR of micro
holes with above electrolyte is increased by 35%. Meanwhile, the composite electrolyte maintains its good machining localization and being
eco-friendly. No electrolytic products are deposited on the surface of the tool electrode or workpiece. As a result, both machining efficiency
and stability are improved by using the composite electrolyte.
© 2016
2016 The
The Authors.
Authors.Published
PublishedbybyElsevier
ElsevierB.V.
B.V. This is an open access article under the CC BY-NC-ND license
Peer-review under responsibility of the organizing committee of 18th CIRP Conference on Electro Physical and Chemical Machining (ISEM
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
XVIII).
Peer-review under responsibility of the organizing committee of 18th CIRP Conference on Electro Physical and Chemical Machining
(ISEM XVIII)
Keywords: Micro ECM; electrolyte; SS304; complexing agents; sodium citrate.

1. Introduction conductivity. Ultimately, machining efficiency and surface

Stainless steel 304 (SS304) is widely used in industrial
technology fields such as automobile and aerospace due to its
strong corrosion resistance and excellent machining
performance. Currently, the machining requirements of micro
holes and grooves on precision parts are rapidly increased.
Micro electrochemical machining (Micro ECM) has many
advantages such as regardless of mechanical properties of
material, high forming accuracy, good surface quality and
absence of residual stress. It has potential superiority in
machining micro holes even 3D microstructures [1-3].
Therefore. Researches on ECM for micro holes with high
aspect ratio on SS304 have important research value and
application prospects.
During ECM process of micro holes with high aspect
ratio, renewal channel of electrolyte is blocked by electrolytic
products. And the products also result in the fluctuation of
quality of the workpiece are deteriorated. The electrolytic
products adhering to the electrode and workpiece affect
process stability and accuracy at the same time. So far,
researchers propose electrode intermittent retraction method
[4] and micro-helix electrode with high-speed ration method
[5]. Machining efficiency is partly improved by utilizing
above means, respectively. However, there are many
deficiencies through those physical and mechanical ways, as
the aspect ratio is increased. For instance, the revolving rate
of principal axle is too high.
Material removal in ECM is based on the principle of
electrochemical reaction. As a result, electrolyte constituent
plays an important role in ECM. Acidic and neutral
electrolyte are commonly used currently. Micro holes on
SS304 with thickness of 100 μm are obtained by adopting
dilute sulphuric acid [6]. Microstructures on SS304 are
processed with the mixture of HCl and H2SO4 as electrolyte.

2212-8271 © 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of 18th CIRP Conference on Electro Physical and Chemical Machining (ISEM XVIII)
doi:10.1016/j.procir.2016.02.223
 Liu Guodong et al. / Procedia CIRP 42 (2016) 412 – 417
The surface quality of the workpiece is improved significantly
[7]. As for the application of neutral electrolyte, NaClO3 and
NaNO3 solution are employed as electrolyte in ECM [8-9].
Micro holes on 300 μm thick SS304 are achieved. The feed
rate comes within 1~2 μm/s.
According to the above literature, high machining
efficiency could be reached with acidic electrolyte, as well as
good surface quality. However, it is difficult to control
machining localization. Machine tool corrosion and waste
treatment problems are also appeared. By contrast, good
nonlinear characteristics and high machining accuracy can be
achieved by utilizing neutral passive electrolyte. It is easy to
reach good machining localization, whereas the depth of
micro holes is restricted by insoluble electrolytic products.
In order to remove insoluble electrolytic products from
inter-electrode gap in neutral electrolyte, researchers explore a
feasible way as adding additives to electrolyte. The insoluble
electrolytic products could be dissolved through chemical
reactions. The electrolyte containing NaClO3 and ethylene-
diaminetetraacetic acid disodium (EDTANa2) [10] has good
performance for micro holes on SS304 (400 μm thickness).
Electrolytic products deposited on the electrode surface are
reduced because of the complexing effect of EDTANa2.
Consequently, process stability is improved. But machining
efficiency is low with feed rate of 0.25 μm/s. Micro holes on
SS304 with thickness of 100 μm are achieved by using citric
acid as electrolyte [11], which can avoid the formation of
insoluble products. But the machining localization is affected
due to its acidity. The neutral electrolyte adding NaHSO4
emphasizes the same effect [12]. But the acidic property
breaks up the machining accuracy.
Above researches provide a feasible way to solve the
insoluble products removal problem in neutral electrolyte.
Considering the precondition to keep characteristics of neutral
electrolyte with good machining localization and being eco-
friendly, exploration of optimization of composite electrolyte
constituent has to be researched deeply. The experimental
study and theoretical analysis are still lacking.
The selection and optimization of composite electrolyte are
researched in this paper. Complexing agents are utilized to
generate soluble products with metal ions. Based on the
analysis of properties of complexing agents, Micro ECM
experiments on SS304 are carried out. Combined with the
experimental results, products deposition on electrode surface,
inlet diameter, material removal rate (MRR), ratio of removal
rate to current (MRC), etc. are taken as evaluation criterions to
optimize electrolyte constituent. Consequently, the machining
accuracy, efficiency and process stability of ECM for micro
holes with high aspect ratio could be improved.
2. Role of complexing agents in electrochemical reaction
2.1. Reaction mechanism of complexing agents
Complexing agents are utilized to generate soluble
products with metal ions. The schematic diagram of
electrochemical reactions with complexing agents is shown as
Fig. 1.
413
Fig.1. Schematic diagram of electrochemical reactions
The anode metal (workpiece) is oxidized into metal ions
Mn+. Further it generates hydroxide precipitate with OH- in
neutral electrolyte as equation (1) and hydrogen is also
generated. In the case of adding complexing agents, ligand L
in complexing agents would contend with OH- and O2 for Mn+
to generate clathrate as equation (2), which is soluble in water.
The ligand L could be with negative charge or with no charge.
The number of the charge is ignored.
M  nOH o M(OH)n p (1)
Mn++aL ↔ MLa (2)
The competitive reaction between clathrate generation
and hydroxide dissolution is shown as equation (3).
M(OH)n+aL↔MLa+nOH- (3)
The competition coefficient [13] of clathrate generation
is as follows:
[MLa ] u [OH- ]n
Kj= =Ksp (M(OH)n ) u K f (MLa ) (4)
[L]a
Where Ksp (M(OH)n) denotes the solubility product of
M(OH)n in water. Kf(MLa) is the stability constant logarithm
of clathrate MLa. The stronger complexing ability of
complexing agents, the more stable of the generated clathrate
under the same condition. In other words, the greater is Kf
value, the greater is Kj value. So hydroxide precipitate could
be dissolved smoothly with strong complexing agents. It
attributes to remove the insoluble products.
2.2. Physical and chemical properties of complexing agents
The kinds and properties of complexing agents in
electrolyte play an important role for dissolving capacity to
precipitate. The property such as strong complexing ability,
high solubility in water, small viscosity, stable structure are
required. Considering the physical and chemical properties,
complexing agents whose ligand structure contains
polyhydroxy acid group, alcamines group and complexone
could be adopted as additive in electrolyte.
The ligand structure of polyhydroxy acid group is shown
as Fig. 2a. The –OH and –COO- are contained. Under the
condition of being neutral, O atoms on –COO- participate in
complexing reaction. Complexing ability of those complexing
agents is strong. Meanwhile, the hydrophilic group –OH
makes the generated clathrate have high solubility in water.
The ligands structure of alcamines group is shown as Fig. 2b.
414 Liu Guodong et al. / Procedia CIRP 42 (2016) 412 – 417
H atoms on amino are partially ionized and mixed clathrate
could be generated with OH-. The structure of complexone is
shown as Fig. 2c. The O atoms on both N atoms and –COO-in
the structure could participate in complexing reaction.
Therefore, its complexing ability is very strong. And stable
chelates could be generated.
Fig. 2. Chemical structural formula of three kinds of ligands
Considering the properties and complexing ability. The
complexing agents are preliminary screened in the above
analysis. However. The electrochemical reaction and
influence factors in ECM are very complicated. So the
selection of electrolyte constituent must refer to the
experimental results.
3. Selection and optimization method of composite
electrolyte for Micro ECM
As for the selection and optimization of composite
electrolyte for Micro ECM, the evaluation criterions for good
machining performance are proposed combined with
experimental results. The optimal electrolyte is gained by
three steps as selecting the primary electrolyte, optimizing
concentration and selecting the complexing agents. The
schematic diagram of selection and optimization for
composite electrolyte constituent is shown in Fig. 3.
Fig. 3. Schematic diagram of composite electrolyte optimization
3.1. Evaluation criterions for electrolyte optimization
Considering among machining localization, machining
efficiency and surface quality at the same time, the optimal
electrolyte constituent is selected. However, evaluations of
above machining performances are abstract. Moreover the
experimental data cannot present them perfectly. It is
important to choose experimental results as evaluation
criterions to evaluate the machining performance. Ultimately,
the optimal composite electrolyte is obtained by overall
considering the criterions.
As shown in Fig. 3. Inlet diameter reflects the stray
corrosion with the electrode feeding, namely the machining
localization. Increase rate of material removal rate (IRMRR) is
used, whose physical meaning is the increase coefficient of
MRR with complexing agents (with L) compared to MRR
with pure primary electrolyte (without L). Its expression is
shown as equation (5). As a result, both MRR and IRMRR
reflect the machining efficiency. The largest feed rate reflects
process stability of ECM process. In other words, the more
stable of ECM process, the larger feed rate could be reached
under the same condition.
MRR with L - MRR without L
IR MRR = u 100% (5)
MRR without L
Electrolytic products in inter-electrode gap would
deposit on the electrode surface and the side wall of holes,
which adversely influence the process stability of ECM. The
products deposition condition on electrode surface can
reflect process stability and surface quality of the workpiece.
Meanwhile, the entrance circular degree and contour shape
of micro holes present shape accuracy. In order to study the
material removal of workpiece under a certain current
conditions, we define the ratio of removal rate to current
(MRC) to reflect the match performance of materials with
electrolyte. In brief, MRC is the MRR of workpiece under
certain current of 1 A, whose expression is shown as
equation (6). The current I is measured by the power supply
automatically. Its physical meaning is the amount of energy
which consumes for material removal in ECM process. In
other words, the larger MRC value under the same
conditions, better match performance of materials with
electrolyte. Current efficiency and machining efficiency are
improved with high MRC value.
MRR
MRC= (6)
I
3.2. Selection of primary electrolyte and concentration
It is more difficult to remove insoluble products of micro
holes with high aspect ratio (compared with micro groves). In
this study, ECM experiments of micro holes are carried out on
SS304 to illustrate the influence of insoluble products.
Machine tool prepared by ourselves is adopted as an
experimental device. High-frequency pulse power supply
outputs the pulse current [14]. The micro hollow electrode is
used as a tool electrode with outer diameter of 130 μm, inner
diameter of 65 μm and length of 3.5 mm [15]. The electrolyte
flow through the electrode is achieved by high pressure liquid.
Neutral salt solution is selected as the primary electrolyte
considering the environmental protection. Neutral electrolyte
such as NaNO3, NaClO3 and NaCl are commonly used. Micro
holes are obtained on SS304 of 500 μm thickness with above
electrolyte, respectively. The experimental parameters are
shown in table 1.
Table 1. Micro ECM process parameters
Process parameters Value
Voltage (U / V) 8
Pulse width (Ton / μs) 5
Interpluse width (Toff / μs) 5
Inflow pressure (P/ MPa) 0.55
 Liu Guodong et al. / Procedia CIRP 42 (2016) 412 – 417
Considering the thickness of workpiece and the aspect
ratio of holes, the target dimension of micro hole is selected
as inlet diameter of 160~190 μm. The relationship between
MRR, inlet diameter with feed rate is shown in Fig. 4.
Fig. 4. Relationship between MRR, inlet diameter with the feed rate
MRR achieved in ECM experiments with NaNO3 and
NaClO3 solution as electrolyte are almost equivalent (about
7.5×10-4mm3/s). The inlet diameter range of holes with
NaNO3 is 157 ~ 218 μm, which meet the demand of the target.
The corresponding diameter of NaClO3 is 208 ~ 249 μm.
MRR reached with NaCl as electrolyte is larger than above
(13.5×10-4mm3/s). However, the inlet diameter is larger than
320 μm. Utilizing the evaluation criterions of primary
electrolyte, NaNO3 solution is selected as the primary
electrolyte in later ECM experiments.
The relationship of inlet diameter with feed rate using
different concentrations of NaNO3 solution is shown in Fig. 5.
The largest feed rate reaches 15μm/s with electrolyte
concentrations of 1.5 mol/L. But the corresponding inlet
diameter is larger than 195 μm. The largest feed rate with 0.25
and 0.5 mol/L NaNO3 are lower (<7 μm/s), namely, the
corresponding process stability are worse. Inlet diameter of
1.0 mol/L NaNO3 is in the range of 169 ~ 215 μm and the
largest feed speed is 12 μm/s, which meet the demand of the
target. Taking into account the evaluation criterions of
primary electrolyte concentration, the optimal electrolyte
concentration of NaNO3 solution is 1.0 mol/L.
Fig. 5. Relationship between inlet diameter and feed rate
3.3. Optimization of complexing agents
Complexing agents contain three kinds of ligand
structures described in section 2.2 are used in ECM
415
experiments. As for complexing agents with polyhydroxy acid
group, sodium citrate (Na3Cit), sodium tartrate (Na2Tart) and
sodium gluconate (NaGlu) are the representatives.
Triethanolamine (Tea) which contains alcamines group is
chosen as complexing agents. Ethylenediaminetetraacetic acid
disodium (EDTANa2) is selected as a kind of complexone.
Above complexing agents react with Fe3+, Fe2+ and Ni2+
from SS304. Different clathrates are generated and the
stability of them is various. Consequently, hydroxide
participate dissolving capacity of them is various. Under the
condition of PH = 7, taking Fe(OH)3 dissolution as an
example, the competition coefficient logarithm lgKj is shown
in table 2.
Table 2. Competition coefficient logarithm lgKj value of above complexing
agents for Fe(OH)3[16]
Complexing agents lgKj
Na3Cit -9.6
Na2Tart -19.1
NaGlu -26.0
Tea -16.8
EDTANa2 -11.4
Utilizing 1.0 mol/L NaNO3 with 0.01 mol/L above
complexing agents, ECM experiments of micro holes are
carried out. Experimental parameters are shown in table 1.
The case with no additive and adding H2SO4 (PH = 5) is set as
comparison experiments.
Inlet diameter and IRMRR with different composite
electrolyte are shown in Fig. 6. IRMRR with EDTANa2 and Tea
in the electrolyte is increased by 22% and 10%, respectively.
The corresponding range of inlet diameter is 200 ~ 215 μm.
IRMRR with Na3Cit, Na2Tart and NaGlu in electrolyte
increased by 35%, 34% and 43%, respectively. The
corresponding range of inlet diameter is 178 ~ 195 μm. It
demonstrates that the machining efficiency improved
significantly with complexing agents with Na3Cit, Na2Tart
and NaGlu in electrolyte (>34%). And the inlet diameter
meets the demand of the target. The composite electrolyte
with these three complexing agents have good machining
performance.
Fig. 6. Inlet diameter and IRMRR with different complex electrolyte
Surface condition of electrode and workpiece with pure
NaNO3 electrolyte is shown in Fig.7. Among which, Fig. 7a,
416 Liu Guodong et al. / Procedia CIRP 42 (2016) 412 – 417
7b show the products deposition of the entrance and exit of
the hole respectively. And Fig.7c shows the state of the
electrode surface. There are some electrolytic products.
Fig. 7. Surface of workpiece and electrode with NaNO3 electrolyte
Fig.8a, 8b show the results of adding H2SO4 electrolyte.
It demonstrates that no products is deposited on the surface of
workpiece and electrode with adding H2SO4 electrolyte. But
the circular degree and edge profile of holes are very poor.
Fig.8c~8f show the corresponding holes and surface condition
of the electrode with adding Na3Cit and NaGlu composite
electrolyte. No products are deposited on the surface of the
electrode or workpiece and the circular degree of entrance is
good. The edge profile is clear as well.
Fig.8. Surface condition of workpiece and electrode with +H2SO4, +Na3Cit
and +NaGlu composite electrolyte
The corresponding holes and surface condition of
electrode with adding Na2Tart and Tea composite electrolyte
are shown in Fig.9a~9d. There is a mass of electrolytic
products on tool electrode and workpiece surface. And the
edge profile is hazy. Fig. 9e, 9f show the corresponding holes
and tool electrode surface condition with adding EDTANa2 in
electrolyte. Workpiece and the electrode surface have no
products deposited. The circular degree of entrance is good.
The composite electrolyte with Na3Cit, NaGlu and EDTANa2
as complexing agents have good machining performance.
Fig.9. Surface condition of electrode and workpiece with +Na 2Tart, + Tea and
+ EDTANa2 composite electrolyte
Fig.10 shows the comparison of MRC with various
composite electrolyte. The results reveal that the maximum
MRC value of 479.5 μm3/A·s is obtained with Na3Cit as
complexing agents. It increases by 2 times compared to pure
NaNO3. MRC value of NaGlu is in the second position. In
other words, the current efficiency with Na3Cit is the highest.
Anode material removal in this process is stable. The match
performance of SS304 and composite electrolyte with Na3Cit
is the best. So composite electrolyte with Na3Cit have good
machining performance.
Fig. 10. Comparison of MRC value of different composite electrolyte
As the machining performances like localization,
machining efficiency, process stability, match performance of
materials and electrolyte are considered. Sodium citrate is
selected as complexing agents in composite electrolyte.
The composite electrolyte used for SS304 is optimized as
1.0 mol/LNaNO3 + 0.01 mol/L sodium citrate. Ultimately, the
micro holes with high aspect ratio can be obtained on SS304
with diameter of 160~190 μm. The feed rate is about 12 μm/s.
And machining efficiency and process stability are improved
significantly.
4. Experimental Results discussion
Under the condition of electrolyte being neutral, the
complexing agents containing polyhydroxy acid group
(Na3Cit, Na2Tart, NaGlu) have strong complexing ability to
dissolve insoluble products. It results in very high IRMRR (>
35%) than others. The quantity of hydrophilic group –OH in
NaGlu is the most, which results in the largest solubility of
the generated clathrate. The MRR with NaGlu in composite
electrolyte is significantly improved [16]. So the highest
machining efficiency is achieved with NaGlu. The
concentration of COO- in Na3Cit is the largest. Consequently,
the ligands can react with Fe2+ and Ni2+, which promote the
reaction Fe  2e o Fe2 . The energy consumed in this reaction
is less than the generation of Fe3+. So the MRC value is higher
than others with Na3Cit.
The surface activity of the generated clathrate is weak by
using Na3Cit and NaGlu as additive. That means, the adhering
effect on metal material is weak. In other words, no products
are deposited on the electrode and workpiece surface.
However, due to the symmetrical structure of Na2Tart with
two –OHs, the mixed chelate is generated with tartrate acid
root as the bridge group. It leads to stronger adhering effect.
Therefore, electrolytic products are deposited on the electrode
and workpiece surface with Na2Tart as additive.
The complexing capability of Tea is strong, whereas the
generated clathrate have distinct adhering effect on the metal
material because of its strong surface activity. Therefore,
there is a large amount of electrolytic products on electrode
and workpiece surface. Ultimately, it affects process stability
 Liu Guodong et al. / Procedia CIRP 42 (2016) 412 – 417
and shape accuracy.
The complexing capable of EDTANa2 is very strong
(lgKj=-11.4). So the removal of insoluble electrolytic products
could be achieved smoothly. Furthermore, the structure of
generated chelate is stable and its adhering effect is weak. So
there are no products on the electrode and workpiece surface.
The molecular volume of the chelate generated by EDTA2-
ligand and metal ions is large, which causes slower diffusion
rate in electrolyte. It results in the concentration polarization.
Finally machining efficiency and process stability are
deteriorated. Therefore it results in lower IRMRR (10%) and
poor process stability.
It is verified that complexing ability is an important
factor for selecting complexing agents according to the
experimental results. But the structural properties of ligand
(e.g. Na2Tart), surface adhering effect of the generated
clathrate (e.g. Tea), and the molecular volume (e.g. EDTANa2)
should be taken into account. So experimental verification is
necessary based on the theoretical analysis when select the
optimal composite electrolyte constituent.
5. Conclusion
Based on the analysis of the reaction mechanism with
complexing agents in ECM, the experiments of micro holes
on SS304 are carried out. Combined with the experimental
results, the electrolyte constituent is selected and optimized.
Finally, the reaction characteristic and experimental
phenomena are discussed. The main conclusions can be
obtained as follows:
x Composite electrolyte containing neutral salt solution and
complexing agents is adopted. The complexing agents in
electrolyte compete for metal ions to dissolve the insoluble
electrolytic products. It is verified to be effective to
increase the machining depth of micro holes in ECM.
x The selection and optimization of composite electrolyte
constituent are employed for good performance in ECM.
Products deposition on the electrode surface, inlet diameter,
MRR, MRC are taken as evaluation criterions. The
machining accuracy, efficiency and process stability are
overall considered. Consequently, the optimal composite
electrolyte constituent is obtained.
x The composite electrolyte used for SS304 is optimized as
1.0 mol/LNaNO3 + 0.01 mol/L sodium citrate. MRR of
ECM with electrolyte containing Na3Cit is increased by
35% compared to pure NaNO3 and MRC increases by 2
times. No products are deposited on the surface of the
electrode and workpiece.
Under the precondition for maintaining good machining
localization and being eco-friendly, the machining
417
performance of ECM for micro holes with high aspect ratio is
significantly improved.
Acknowledgements
This research is supported by National Natural Science
Foundation of China (Grant No. 51275255) and Digital
Electrochemical Machining Key Lab of Jiang Su Province
(Changzhou Institute of Technology) Open Foundation (Grant
No. KFJJ2004005).
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