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Journal of the Taiwan Institute of Chemical Engineers 000 (2015) 1–5

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Journal of the Taiwan Institute of Chemical Engineers

journal homepage: www.elsevier.com/locate/jtice

Particle removal performance and its kinetic behavior during oxide-CMP

wastewater treatment by electrocoagulation
Yi-Hung Liu a,b,∗, Chyun-Yaw Lin a, Jui-Hsiung Huang a, Shi-Chern Yen a
a
Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan
b
Department of Greenergy, National University of Tainan (NUTN), Tainan 70005, Taiwan

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

Article history: The treatment of chemical mechanical polishing (CMP) wastewater was investigated using the electroco-
Received 22 April 2015 agulation (EC) method with a focus on its particle removal efficiency and kinetic behavior. The sacrificial
Revised 27 November 2015
electrode for use in the EC treatment was made of Fe, in which the supporting electrolytes of Fe2+ can be
Accepted 29 November 2015
electrolytically generated. Several significant factors including pH, aeration and current density of the treat-
Available online xxx
ment system were evaluated. The experimental results showed that the pH controlled at 5 ∼ 7 after the EC
Keywords: treatment is preferable and applying aeration during the EC is effective for enhancing the particle removal
CMP wastewater efficiency. In this system, the particle removal efficiency was found to achieve 99% by treating the wastewa-
Electrocoagulation ter at a current density 5.9 mA/cm2 in 10 mins. Furthermore, a kinetic reaction model considering the charge
Particle removal efficiency neutralization and particle coagulation was proposed to describe the particle removal mechanism. The cal-
Kinetic behavior culated result based on the model showed good agreement with the experimental data. It was also found
that the reaction orders for the particle and Fe2+ concentration terms in the proposed particle removal rate
equation are 2 and 4, respectively.
© 2015 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction ical method based on the mechanisms of electrodecantation and elec-

For the semiconductor manufacturing process, planarization is a
significant step to obtain a uniform flatness over an integrated circuit
(IC) device. Chemical mechanical polishing (CMP), a planarization
technique developed by IBM in 1985, has been utilized for decades
due to its high polishing capability of increasingly complicated IC de-
vices. Since the slurry used for the CMP process contains fine abra-
sives and chemical compounds, a large quantity of ultrapure water is
thus needed to remove the slurry after polishing [1]. This indicates
that the post treatment of CMP wastewater is an urgent issue regard-
ing the limited use of water resources [2].
Ultrafiltration had been employed for the solid–liquid separation
of CMP wastewater [3], but its efficacy seems to be limited due to se-
vere fouling of the membrane. To avoid this problem, conventional
chemical coagulation combined with reverse osmosis had also been
adopted for the CMP wastewater treatment [4]. Particles can be re-
moved to a certain level; however, the conventional chemical co-
agulation is still not an ideal treatment method due to the specific
wastewater characteristics such as highly-dispersed nanosized parti-
cles and wide pH variations. Belongia et al. proposed an electrochem-
∗ tling and flotation of the pollutants [14]. In addition, they pointed
Corresponding author. Tel.: +886 6 2606186; fax: +886 6 2602205.
E-mail addresses: yhliu@mail.nutn.edu.tw (Y.-H. Liu), scyen@ntu.edu.tw (S.-C. Yen).
trocoagulation (EC) to remove the dispersed particles of silica and
alumina in the CMP wastewater [5]. For the EC treatment, sacrificial
anodes made of iron or aluminum are commonly used to continu-
ously generate metallic ions. These ions can not only neutralize the
negative charge carried by the dispersed particles, but also react with
hydroxyl ions around the anode to form metallic hydroxides capable
of trapping the destabilized particles. A schematic diagram of a typ-
ical EC occurring around an iron electrode is shown in Fig. 1. These
specific reaction mechanisms also enable the EC to be used in many
wastewater treatment processes such as urban wastewater [6], textile
wastewater [7], oil-containing wastewater [8], and wastewater with
arsenic contaminants [9].
For the dynamic coagulation mechanism, three stages including
the lag stage, reactive stage, and stable stage occurring in an EC pro-
cess were previously reported [10]. The dynamic nature of a batch
EC system for treating CMP wastewater has also been investigated
by taking into consideration the aforementioned three stages [11,12].
To predict the particle coagulation behavior during an EC treatment
of a kaolin clay suspension, Matteson et al. proposed a second-order
kinetic model describing the electrophoresis and charge neutraliza-
tion [13]. Holt et al. reported another dynamic model linearly com-
bining two first-order equations related to the behaviors of the set-
out that the main reaction mechanism would shift from flotation to

http://dx.doi.org/10.1016/j.jtice.2015.11.023
1876-1070/© 2015 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Please cite this article as: Y.-H. Liu et al., Particle removal performance and its kinetic behavior during oxide-CMP wastewater treatment by
electrocoagulation, Journal of the Taiwan Institute of Chemical Engineers (2015), http://dx.doi.org/10.1016/j.jtice.2015.11.023
JID: JTICE
ARTICLE IN PRESS
2 Y.-H. Liu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2015) 1–5
Fig. 1. Schematic diagram of particle destabilization by EC method using Fe as a sacri-
ficial electrode.
sedimentation in the case of an evolved gas at the electrodes. The pre-
viously proposed kinetic models enabled a general prediction of par-
ticle loss in the suspension. However, the kinetic reaction mechanism
between the dispersed particles and supporting electrolytes corre-
sponding to the initial charge neutralization and subsequent particle
coagulation is still not well explained.
In this study, CMP wastewater was treated by the EC method with
a focus on the particle removal performance and its kinetic behavior.
Several significant factors including pH, aeration, and current den-
sity were experimentally investigated in order to improve the particle
removal efficiency. For clarifying the reaction mechanism between
the dispersed particles and supporting electrolytes, a kinetic reaction
model was proposed and verified with the experimental results.
2. Experimental
For preparing the CMP wastewater, a slurry (Semi-Sperse® 25
slurry, Cabot Microelectronics Corp., USA) was diluted using deion-
ized water with a volume ratio of 1:100 in order to approximate the
real CMP wastewater used in the semiconductor industries. The pre-
pared wastewater was treated by the EC method in a cylindrical bath
containing ca. 800 cm3 of solution. This EC bath was made of stain-
less steel with an inner iron cylinder that functioned as a sacrificial
electrode, as shown in Fig. 2.
The iron cylinder and stainless steel hollow cylinder were con-
nected to the positive and negative output sides of a DC power sup-
ply (6634B, Agilent) system, respectively. The iron electrode was im-
mersed in a 3 M HCl solution for 3 mins before performing the EC
treatment in order to enhance pitting corrosion [15,16] and prevent
passivation formation [8]. In addition, an air pump used for aeration
was connected to the bottom portion of the bath. The flow rate for
the aeration was controlled at ca. 50 cm3 /s. After the EC treatment,
the wastewater was poured into a beaker and allowed to settle for
10 mins in order to separate the liquid and precipitate. The super-
natant liquid was used for the experimental analysis.
Please cite this article as: Y.-H. Liu et al., Particle removal performance and its kinetic behavior during oxide-CMP wastewater treatment by
electrocoagulation, Journal of the Taiwan Institute of Chemical Engineers (2015), http://dx.doi.org/10.1016/j.jtice.2015.11.023
[m5G;December 18, 2015;16:23]
7.3 cm
2.5 cm
Anode 21.6 cm - +
Power supply
Cathode
CMP suspension
Air
Fig. 2. Experimental EC apparatus for CMP wastewater treatment.
The particle size and zeta potential distributions of the dispersed
particles in the CMP solution were determined using a particle size
and zeta potential analyzer (Zetasizer Nano ZS, Malvern Instruments,
Inc.) based on the dynamic light scattering theory and laser Doppler
effect, respectively. The turbidity was used as an index of the par-
ticle concentration and it was measured by a turbidimeter (2100AN,
HACH). For measuring the pH of the wasterwater, a pH meter (SP-701,
Suntex) was utilized. To invesitgate its effect on the particle removal,
the pH was adjusted by using H2 SO4 (0.1 M) and NaOH (0.5 M) so-
lutions before and after the EC treatment. The amount of residual
Fe after the EC was determined by an inductively coupled plasma
analysis (3100XL, Perkin-Elmer). In addition, all the experiments and
measurements were conducted at room temperature (∼25 °C) and
1 atm.
3. Results and discussion
3.1. Physical properties of prepared CMP wastewater
Fig. 3 shows the cumulative particle size distribution and zeta po-
tential distribution of the prepared CMP wastewater. The particle size
is distributed in a unimodal and symmetrical manner with a narrow
size variation from the median particle size of ca. 90 nm. The zeta po-
tential distribution also seems to be symmetric and the mean value
is ca. –38.8 mV. According to these uniform and small particle sizes,
it is known that the particles in the prepared wastewater should be
well stabilized. The conductivity, total solids, and pH of the prepared
wastewater were also determined to be as 170 μS/cm, 2500 mg/L,
and 9.9, respectively. These results indicate that the physicochemical
properties of the prepared CMP wastewater are very similar to the
real ones [12,17].
3.2. pH effect on particle removal
The effect of the pH on the particle removal after the EC treatment
is shown in Fig. 4. The particle removal efficiency, η, is determined by
the following equation:
η (% ) = (T0 − T )/T0 × 100 (1)
where T0 and T represent the initial turbidity and the turbidity after
the treatment, respectively. The turbidity significantly decreases as
the pH is increased from 4 to 5 and a minimum value of 0.5 NTU can
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Y.-H. Liu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2015) 1–5 3

Fig. 3. Cumulative particle size distribution (a) and zeta potential distribution (b) of the prepared CMP wastewater.

200 100 60
Particle removal efficiency, η (%)

80 40
150
Zeta potential (mV)
Turbidity (NTU)

20
60
100 0
40
-20
50
20
-40
0 0
4 5 6 7 8 9 10 -60
2 4 6 8 10
pH
pH
Fig. 4. Effect of pH on particle removal after EC treatment. (treatment conditions:
5.9 mA/cm2 for 10 mins with aeration). Fig. 5. Relationship between zeta potential of particles and pH.

be obtained at pH 6. However, the turbidity tends to increase again

with the increasing pH until 10. It was found that the pH range for a
particle removal efficiency above 95% is 5 ∼ 7. According to the Pour-
baix diagram of Fe, metal ions (Fe3+ or Fe2+ ) tend to be present not
only in an acidic environment, but also in a basic environment with a
higher oxidation potential. On the other hand, the hydroxide (Fe(OH)3
or Fe(OH)2 ) tends to form at a medium pH with an oxidation state.
The hydroxide formed around the anode is thus stable at pH 5 ∼ 7,
corresponding to the higher particle removal efficiency. This result
also shows a good agreement with the design-and-operation diagram
for the ferric chloride coagulant in the literature [18], reporting that
the formed hydroxide in this pH range tends to trap the destabilized
particles, resulting in a sweep coagulation.
Fig. 5 shows the variation in the zeta potential of particles versus
pH of the prepared wastewater containing Fe ions. The zeta poten-
tial tends to be positive in an acidic environment; while it tends to
be more negative in a basic environment. Therefore, the isoelectric
point should be present at pH 5 ∼ 6. This result can also account for
the higher particle removal efficiency shown in Fig. 4, since a lower
zeta potential in this pH range is advantageous for the particle desta-
bilization.
A similar pH adjustment was also carried out before the EC treat-
ment, while no obvious effect on the particle removal efficiency was
found. Based on these results, the pH was controlled at 6 after all the
EC treatments in the following experimental investigations.

Please cite this article as: Y.-H. Liu et al., Particle removal performance and its kinetic behavior during oxide-CMP wastewater treatment by
electrocoagulation, Journal of the Taiwan Institute of Chemical Engineers (2015), http://dx.doi.org/10.1016/j.jtice.2015.11.023
 JID: JTICE
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4 Y.-H. Liu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2015) 1–5

and it is ca. 100% as the current density reached 5.9 mA/cm2 . This
means that a larger amount of released ions is needed to effectively
complete the particle removal, which is also in consistent with the
result of a previous study [17]. Meanwhile, the residual Fe content in
the supernatant shows the opposite tendency with a concentration
of less than 1 ppm at the highest current density. This indicates that
the released ions, approximately 3.1 × 10−3 mol from a preliminary
calculation, are more sufficient at the highest current density, being
able to electrostatically interact with the particles and effectively re-
act with the hydroxyl ions to form a hydroxide. As a result of the
sweep coagulation, a higher particle removal efficiency is achieved
and lower residual Fe remained in the supernatant due to the effi-
cient consumption of the released ions.

3.4. Reaction mechanism and kinetic reaction model

Fig. 6. Time course of particle removal efficiency regarding the influences of aeration
and current density. (case (a): aeration applied at 5.9 mA/cm2 ; case (b): aeration ap-
plied at 2.9 mA/cm2 ; case(c): no aeration applied at 5.9 mA/cm2 ).
Generally, the dispersed particles in the CMP wastewater possess
strong electrostatic charges, inducing an electrostatic repulsive force
between the particles. An energy barrier preventing particle coagu-
100 20 lation is thus formed due to the repulsive force, leading to a stabi-
Particle removal efficiency, η (%)

lized suspension. Once the energy barrier is overcome by an extra en-

ergy resulting from the electrical attraction and Brownian movement,
95 15
Residual Fe (ppm)
particle coagulation can occur. Based on the theoretical concept, we
first postulate that if a suspension is well-stirred, the dispersed par-
90 10 ticles can frequently encounter the released ferrous ions to rapidly
form the intermediate particles through the double layer compres-
sion and electrical neutralization. In the meantime, the ions can also
85 5 move away from the particles due to thermal motion, fluctuation, and
hydration. Thus, a reversible reaction, which describes the aforemen-
tioned behaviors between the particles and ions, can be expressed as
80 0 follows:
0 1 2 3 4 5 6 7
k1 ,k−1
Current density (mA/cm2) P + mFe2+ ←→ (P−mFe2+ ) (2)

Fig. 7. Effect of current density on particle removal efficiency and residual Fe content.
where P, m, P-mFe2+ represent the dispersed fine particles, the sto-
(treatment conditions: 10 mins with aeration applied). ichiometric number of ferrous ions, and the intermediate particles,
respectively.
Since the repulsive force between the intermediate particles is
3.3. Aeration and current density effects on particle removal overcome by the ions, they can further react with each other to form
large-size particles, i.e., coagulation, due to a dominant van der Waals
Fig. 6 shows the time course of the particle removal efficiency force, which can be shown by Eq. (3).
regarding the influences of the aeration and current density. The k2
n(P − mFe2+ ) −
→ PL (3)
removal efficiency reaches almost 100% after a 3-min treatment at
5.9 mA/cm2 with aeration (a). When the current density decreased to where n and PL represent the stoichiometric number of intermediate
2.9 mA/cm2 , a longer treatment time (10 mins) was needed to reach particles and the larger-size particles, respectively.
a removal efficiency above 95% (b). For the case without aeration (c), If the reaction rate between the particles and ions in Eq. (2) is suf-
the removal efficiency begins to increase after a time lag and is lower ficiently high to reach equilibrium and the rate-determining step for
than 90% even after a 10-min treatment despite the application of the particle destabilization is assigned to Eq. (3), then the equilibrium
the higher current density of 5.9 mA/cm2 . Applying aeration to an EC constant and the rate equation of the dispersed particle concentra-
system can improve the mass transport of the dispersed particles, ef- tion can be respectively expressed as follows:
fectively enhancing the mixing of the released ferrous ions and the C(P−mFe2+ )
particles. Accordingly, the particles in case (a) can be rapidly destabi- K= (4)
CP · CFe
m
2+
lized with the release of sufficient ferrous ions, resulting in favorable
particle removal efficiency. In the meantime, fouling on the electrode dCP /dt = −k2C(nP−mFe2+ ) (5)
surface can also be avoided by the aeration effect, which is beneficial
for particle removal. This is also reasonable for case (b) in order to where CP , CFe 2+ and C(P- m Fe 2+ ) are the concentrations of the dis-
achieve the same level of removal efficiency on a longer time scale persed particles, ferrous ions, and intermediate particles, respec-
due to a slower ion release rate. On the other hand, for case (c), the tively.
diffusion rate of the released ions may not be sufficient to affect the By replacing C(P- m Fe 2+ ) in Eq. (5) with the equilibrium constant,
particles in order to complete the particle destabilization in the first the rate equation can be further described as follows:
2 mins. Despite the removal efficiency increases after 3 mins, the lim- dCP /dt = −k2 K nCPnCFe
nm  n nm
2+ = −K CP CFe2+ , (6)
ited mass transport of the ferrous ions and the electrode fouling may
where K is k2 ·Kn .
result in a poorer particle removal efficiency in the EC system without
Meanwhile, the rate equation for ferrous ion concentration can be
aeration.
expressed as:
Fig. 7 shows the effect of the current density on the particle re-
moval efficiency and residual Fe content. In this 10-min treatment, iAe
dCFe2+ /dt = − mK CPnCFe
nm
2+ (7)
the removal efficiency is improved by increasing the current density 2FV

Please cite this article as: Y.-H. Liu et al., Particle removal performance and its kinetic behavior during oxide-CMP wastewater treatment by
electrocoagulation, Journal of the Taiwan Institute of Chemical Engineers (2015), http://dx.doi.org/10.1016/j.jtice.2015.11.023
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4. Conclusions

The CMP wastewater treatment using the EC method was ex-

Fig. 8. Experimental and calculated results of time course of normalized particle con-
centration (calculated data are expressed in lines as a parameter of K ).
Table 1
Constants used in theoretical calculation.
perimentally and theoretically investigated. After the EC treatment,
the pH controlled at 5 ∼ 7 was preferred because the formed
hydroxide can effectively trap the destabilized particles, improv-
ing the effective particle removal. Aeration was found to accel-
erate the interaction between the released ferrous ions and dis-
persed particles as well as avoid electrode fouling, enhancing the
particle removal efficiency. It was also found that a high particle
removal efficiency of 99% and low residual Fe content less than
1 ppm can be obtained by treating the wastewater at 5.9 mA/cm2
in 10 mins using this system. To describe the destabilization phe-
nomenon, a kinetic reaction model considering the charge neutraliza-
tion and particle coagulation was proposed. Based on this model, the
calculated time course of the particle concentration was in good
agreement with the experimental result, and the reaction orders for
the particle and ferrous ion concentrations were found to be 2 and 4,
respectively.

CP0 Initial particle concentration = 1.66 × 102 (mol/m3 ) Acknowledgment

i Current density = 59 (A/m2 )
Ae Electrode surface area = 1.69 × 10–2 (m2 )
The authors would like to thank Mr. Hong-Shiang Tang of the In-
F Faraday constant = 96485 (C/mol)
V Volume of reaction bath = 8 × 10–4 (m3 ) dustrial Technology Research Institute for his helpful advice and tech-
nical support regarding the experiment.

where i is the current density, Ae is the electrode surface area, F is
Faraday’s constant, and V is the volume of the reaction bath. The first
term on the right side of Eq. (7) represents the production rate of
the ferrous ions released from the sacrificial electrode, while the sec-
ond term is regarded as the consumption rate of the ions due to the
particle destabilization, which is m times the rate for the dispersed
particles. The production rate of the ions is considered much higher
than the consumption rate dominated by the collision probability of
the particles and the ions; therefore, the second term of Eq. (7) can
be neglected and the concentration can be analytically obtained as:
 
iAe
CFe2+ = ·t (8)
2FV
Next, by substituting Eq. (8) into Eq. (6), an analytical expression
for the particle concentration profile could be deduced as follows:
 nm
iAe t (nm+1)
1/ = 1 + Cp0 K  · (9)
2FV nm + 1
where  is CP /CP0 , which represents the dimensionless particle con-
centration.
The calculated time course of the normalized particle concentra-
tions based on Eq. (9) is compared with the experimental one, as
shown in Fig. 8. The experimental result from case (a) of Fig. 6 is
shown. The constants used for the calculation are listed in Table 1.
The calculated concentration decays in a similar trend as the experi-
mental one, exhibiting a reactive stage for rapid particle removal [10].
A best-fit profile can be found for n = 2, m = 2, and K = 0.26, indicat-
ing that the reaction order for the particle and ferrous ion concentra-
tions in Eq. (6) are 2 and 4, respectively. Based on this result, it should
be noted that the particle destabilization in the EC system can be ini-
tiated by the formation of the intermediate particles composed of the
dispersed particles and ferrous ions with a stoichiometric ratio of 2.
Furthermore, it is implied that the proposed reaction mechanism can
be applicable when the mass transport of the released ions is signifi-
cantly enhanced due to the aeration effect.
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Please cite this article as: Y.-H. Liu et al., Particle removal performance and its kinetic behavior during oxide-CMP wastewater treatment by
electrocoagulation, Journal of the Taiwan Institute of Chemical Engineers (2015), http://dx.doi.org/10.1016/j.jtice.2015.11.023