Professional Documents
Culture Documents
a
Zhengzhou Railway Vocational & Technical College, Zhengzhou 451460, China
b
College of Materials and Chemistry, China Jiliang University, Hangzhou 310018, China
A R T I C L E I N F O A B S T R A C T
Keywords: Different zinc-manganese phosphate coatings are prepared on the surface of 16Mn steel which are commonly
Zinc-manganese phosphate coating used as construction structure materials. Ultrasonic treatment has been introduced in the process of phosphating
16Mn steel to enhance the corrosion resistance of different zinc-manganese coatings. The experimental results indicate that
Construction structure materials ultrasonic has a certain impact on the surface morphology, thickness, and corrosion resistance of zinc-manganese
Corrosion resistance
phosphate coating, but it has no significant effect on the composition of zinc-manganese phosphate coating. The
Ultrasonic
proper ultrasonic power applied promotes the formation of a zinc-manganese phosphate coating with a compact
surface and large thickness which can effectively block the penetration of corrosive media and enhance the
corrosion resistance. The zinc-manganese phosphate coating prepared using an ultrasonic power of 135 W de
monstrates the best surface density with a thickness of 12.2 µm, and its anti-dripping time, charge transfer
resistance and low-frequency impedance modulus reach 236 s, 5696 Ω cm2 and 4625 Ω cm2, respectively. In
comparison to the zinc-manganese phosphate coating obtained without ultrasonic, the zinc-manganese phos
phate coating prepared with ultrasonic exhibits excellent corrosion resistance and can provide ideal surface
protection for 16Mn steel as construction structure materials.
1. Introduction been done and reported in the lab about the work of ultrasonic-assisted
phosphating. For example, Sun et al. study the effect of ultrasonic on
Phosphating is a widely used surface treatment process for steel. It is the corrosion resistance of phosphate coatings on carbon steel. It is
known that phosphate coating is a functional coating that is non-con found that the ultrasonic phosphate coating can provide an effective
ductive and insoluble in water [1,2]. The bonding strength between the barrier to improve corrosion resistance [7]. Ultrasonic irradiation and
steel and the phosphate coating is very good. Phosphate coatings can be its application for improving the corrosion resistance of phosphate
divided into iron phosphate coating, zinc phosphate coating, zinc-man coatings is reported by the Sheng et al. [8]. Moreover, effect of ultra
ganese phosphate coating, zinc-calcium phosphate coating, and manga sonic waves on the performance of calcium phosphate composite
nese phosphate coating [3,4]. Regardless of the type of phosphate coating is investigated by Fathyunes and Khalili [9]. In order to provide
coating, the corrosion resistance is crucial. Therefore, it is of great sig technical support for the application of phosphate coatings, it is ne
nificant to improve the corrosion resistance of phosphate coating. cessary to investigate the impact of important process parameters such
It is reported that the corrosion resistance of phosphate coatings can as ultrasonic power or ultrasonic frequency on the corrosion resistance
be improved by changing the composition of phosphate solution and of phosphate coatings. In the paper, the 16Mn steel is used as the re
optimizing phosphating parameters [5,6]. Research has also shown that search object, and different zinc-manganese phosphate coatings are
introducing ultrasonic during the phosphating process can also achieve prepared on the surface of 16Mn steel by phosphating process. Ultra
good results to significantly improve the corrosion resistance of phos sonic with different powers are introduced during the phosphating
phate coatings. However, the current research on ultrasonic-assisted process to further improve the corrosion resistance of zinc-manganese
phosphating of steel is still in the exploratory stage. Some works have phosphate coatings.
⁎
Corresponding author.
E-mail address: shangdizhuli45@126.com (Y. Zhang).
https://doi.org/10.1016/j.ijoes.2023.100274
Received 3 May 2023; Received in revised form 28 June 2023; Accepted 2 July 2023
Available online 3 July 2023
1452-3981/© 2023 The Author(s). Published by Elsevier B.V. on behalf of ESG. This is an open access article under the CC BY-NC-ND license (http://creative
commons.org/licenses/by-nc-nd/4.0/).
Y. Zhang, X. Chen and H. Tan International Journal of Electrochemical Science 18 (2023) 100274
Table 1
Chemical composition of 16Mn steel.
Element Mn C Si Cr Cu Ni P S Fe
Mass fraction/% 1.2–1.6 0.13–0.19 0.2–0.6 0.3 0.25 0.3 0.03 0.03 Residual
2. Experimental materials and methods are tested by Parstat 2273 electrochemical workstation. The saturated
calomel electrode is used as the reference electrode, and the platinum
2.1. Materials electrode is used as the auxiliary electrode. The phosphate coating with
size of 1 cm × 1 cm is as the working electrode. The three electrode
The substrate is 16Mn steel, and its chemical composition is shown system is immersed in 3.5 % sodium chloride solution for 1 h to reach
in Table 1. The surface and edges of the sample is polished in sequence steady state, and the electrochemical impedance spectra are tested. The
with different grades of sandpaper (500#, 1000#, 2000#, 3000#) to amplitude of the excitation signal is 10 mV, the starting frequency is
get smooth. After that, the sample is immersed in acetone for chemical 105 Hz, and the ending frequency is 10−2 Hz. The test data is imported
oil removal, and then immersed in 15 % volume fraction hydrochloric into ZsimpWin software to obtain the charge transfer resistance (Rct)
acid for corrosion activation. Finally, the pretreated sample is washed and low-frequency impedance modulus (|Z|0.01 Hz, impedance modulus
with deionized water and dried. at a frequency of 10−2 Hz) to evaluate the corrosion resistance of 16Mn
steel and different zinc-manganese phosphate coatings. In addition,
2.2. Preparation of zinc-manganese phosphate coating 16Mn steel and different zinc-manganese phosphate coatings are im
mersed in 3.5 % sodium chloride solution for 120 h. After that, the
Zinc-manganese phosphate coating is prepared on the surface of samples are cleaned and dried to be observed the surface morphology.
16Mn steel samples by phosphating process. The main composition of
the phosphate solution includes zinc nitrate 32 g/L, zinc oxide 15 g/L, 3. Results and discussion
manganese dihydrogen phosphate 60 g/L, phosphoric acid 75 g/L, ci
tric acid 2 g/L, and nickel nitrate 1 g/L. The beaker containing the 3.1. Surface morphology and composition of different zinc-manganese
phosphate solution is placed in the water bath of the ultrasonic cleaning phosphate coatings
machine, and maintain the temperature of phosphate solution at
60–63 ℃ through water bath heating. During the experiment, the ul Fig. 1 shows the surface morphology of different zinc-manganese
trasonic frequency is constant at 40 kHz. Different zinc-manganese phosphate coatings prepared on the surface of 16Mn steel. Some re
phosphate coatings are prepared respectively by changing the ultra searchers also report the similar surface morphology of phosphate
sonic power (45 W, 90 W, 135 W and 180 W). The time for phosphating coatings [10,11]. It is found that different zinc-manganese phosphate
is 25 min. In addition, a zinc-manganese phosphate coating is prepared coatings completely cover the surface of 16Mn steel, and the applica
without ultrasonic as a comparison. tion of ultrasonic has a certain impact on the surface morphology of
zinc-manganese phosphate coatings. As shown in Fig. 1(b), the surface
2.3. Performance testing of zinc-manganese phosphate coating of the zinc-manganese phosphate coating obtained without ultrasonic
are irregular with cracks. These cracks will become channels for cor
2.3.1. Surface morphology and composition rosive medium to corrode zinc-manganese phosphate coating and in
The surface morphology of 16Mn steel and different zinc-manganese crease its corrosion tendency.
phosphate coatings are observed using EVO MA15 scanning electron The surface density of the zinc-manganese phosphate coating ob
microscopy, and the compositions of different zinc-manganese phos tained with ultrasonic is improved compared to the zinc-manganese
phate coatings are analyzed using an INCA energy spectrometer to phosphate coating obtained without ultrasonic. This is due to the ca
obtain the mass fraction of each element. vitation effect caused by the transmission of ultrasonic in the phosphate
solution, which generates micro jets to enhance the surface activity of
2.3.2. Thickness measurement the substrate and promote the dispersion of phosphate solution, re
The thickness of different zinc-manganese phosphate coatings on sulting in the increasing of active crystal nuclei number and nucleation
the surface of 16Mn steel is measured using a TT260 thickness gauge. density which attributes to the good compactness. The cavitation effect
The substrate 16Mn steel is a magnetic material and the phosphate of ultrasonic has been investigated by some researchers. For example,
coating is a non-magnetic material. When the measuring head of the Wang et al. point out that the cavitation effect of ultrasonic can ac
thickness gauge is in contact with the phosphate coating on the surface celerate the nucleation sites and assist the removal of hydrogen bubbles
of the steel substrate, the measuring head and the steel substrate form a to improve the compactness of coating [12]. Zhang et al. also verify that
closed magnetic circuit. Because the surface phosphate coating will the micro jet produced by the collapse of cavitation bubble and cavi
change the magnetoresistance of the magnetic circuit, the thickness of tation oscillation could promote the dispersion of solution to improve
the phosphate coating can be calculated. The resolution of the thickness compactness [13]. Moreover, it is found that the ultrasonic cavitation
gauge is 0.1 µm. Five areas on each sample are measured and averaged effect can be used to synthesize uniform and compact materials [14].
to reduce error. As shown in Fig. 1(d), the surface density of the zinc-manganese
coating obtained with ultrasonic power of 135 W is the best.
2.3.3. Corrosion resistance testing However, when the ultrasonic power is higher, the overall cracks on
A copper sulfate solution is prepared for dripping testing. The main the surface of zinc-manganese phosphate coating increase. This will
composition is copper sulfate 41 g/L, sodium chloride 35 g/L, and lead to faster invasion of the corrosive medium into the interior of zinc-
0.1 mol/L hydrochloric acid 13 mL/L. A syringe is used to take solution manganese phosphate coating, thereby enhancing the corrosion ten
droplets onto the surface of each sample, and record the time it takes dency. Due to the extremely strong micro jet generated by high ultra
for the droplets to completely change color with a stopwatch, which is sonic power, it hinders the combination of phosphate ions and metal
defined as the anti-dripping time of zinc-manganese phosphate coating. ions to precipitate and crystallize on the surface of 16Mn steel, resulting
The electrochemical impedance spectra of 16Mn steel and different in rough surface with many crystal defects. In addition, when the ul
zinc-manganese phosphate coatings in 3.5 % sodium chloride solution trasonic power is higher, extremely strong shock waves are generated,
2
Y. Zhang, X. Chen and H. Tan International Journal of Electrochemical Science 18 (2023) 100274
a b c
10 μm 10 μm 10 μm
(a) 16Mn steel (b) phosphate coating (without ultrasonic) (c) phosphate coating (45 W)
d e f
10 μm 10 μm 10 μm
(d) phosphate coating (90W) (e) phosphate coating (135W) (f) phosphate coating (180 W)
Fig. 1. Surface morphology of different zinc-manganese phosphate coatings prepared on the surface of 16Mn steel (The acceleration voltage is 10 kV with 1200 times
magnification and 8 mm working distance).
0 36.38 9.2 12.39 39.24 2.79 Fig. 2 shows the thickness of different zinc-manganese phosphate
45 37.17 8.26 12.85 38.54 3.18
coatings prepared on the surface of 16Mn steel. As shown in Fig. 2, the
90 37.8 8.79 13.24 37.86 2.31
135 38.12 9.03 13.57 38.22 1.06
thickness of the zinc-manganese phosphate coating obtained without
180 35.79 8.42 12.16 39.01 4.62 ultrasonic is about 10 µm. The thickness of the zinc-manganese phos
phate coatings obtained with ultrasonic treatment ranges from 9.4 µm
to 12.3 µm. This indicates that ultrasonic has a certain impact on the
resulting in an increase in cracks in the grain growth process. The thickness of zinc-manganese phosphate coatings. The cavitation effect
disordered distribution causes an increase in the surface roughness of caused by ultrasonic transmission in the phosphate solution can pro
zinc-manganese phosphate coating and a decrease in its density. mote the dispersion of phosphate solution and increase nucleation sites.
Table 2 shows the mass fraction of various elements in different As a result, the formation rate of zinc-manganese phosphate coating is
zinc-manganese phosphate coatings prepared on the surface of 16Mn accelerated, resulting in larger thickness.
steel. From Table 2, it can be seen that the composition of different zinc- The thickness of the zinc-manganese phosphate coating obtained
manganese phosphate coatings are all Zn, Mn, P, O, and Fe elements with ultrasonic power of 135 W reaches 12.2 µm. Compared to the zinc-
which are also reported by some researchers [15,16]. The dissociation manganese phosphate coating obtained without ultrasonic treatment,
of zinc nitrate in the phosphate solution generates Zn2+ (see reaction the thickness increases by about 2 µm. However, when the ultrasonic
Eq. (1)), and the multi-level dissociation of manganese dihydrogen
phosphate generates Mn2+and PO43- (see reaction Eq. (2)). The Zn2+ 12.5
combines with PO43- to form Zn3(PO4)2·4H2O precipitation and crys
12.0
tallize on the surface of 16Mn steel. Moreover, Mn2+, Zn2+, and PO43-
combine to form Mn2Zn(PO4)2·4H2O precipitation, which also crystal 11.5
lizes on the surface of 16Mn steel, as shown in reaction Eqs. (3) and (4). 11.0
Thickness/ µm
3
Y. Zhang, X. Chen and H. Tan International Journal of Electrochemical Science 18 (2023) 100274
240 Table 3
230 Corrosion electrochemical parameters obtained according to electrochemical
impedance spectroscopy.
220
Dripping resistance time/ s
Fig. 4. Electrochemical impedance spectra of different zinc-manganese phosphate coatings prepared on the surface of 16Mn steel (The corrosive medium is 3.5 %
sodium chloride solution, the amplitude of the signal is 10 mV and the frequency is ranged from 105 Hz to 10−2 Hz).
4
Y. Zhang, X. Chen and H. Tan International Journal of Electrochemical Science 18 (2023) 100274
accordingly, indicating that the corrosion resistance of zinc-manganese 3.3.3. Corrosion morphology analysis
phosphate coating gradually improves. Fig. 5 shows the corrosion morphology of different zinc-manganese
Based on the above analysis, appropriately increasing the ultrasonic phosphate coatings prepared on the surface of 16Mn steel after im
power can promote the formation of zinc-manganese phosphate coating mersing in 3.5 % sodium chloride solution for 120 h. As shown in
with fewer crystal defects and better surface density to effectively block Fig. 5(a), the corrosion of 16Mn steel is severe after immersing in 3.5 %
the penetration of corrosive medium and increase the resistance to sodium chloride solution for 120 h. The surface is covered with a large
corrosion reactions. The zinc-manganese phosphate coating obtained number of granular and flocculent corrosion products, which is rough
with ultrasonic power of 135 W has the largest capacitive reactance arc and loose. As shown in Fig. 5(b), the zinc-manganese phosphate coating
radius and the highest charge transfer resistance of 5696 Ω cm2, which obtained without ultrasonic also suffer severe corrosion after immersing
is higher than that of the zinc-manganese phosphate coating obtained in 3.5 % sodium chloride solution for 120 h. However, lower amount of
without ultrasonic treatment and 16Mn steel. However, as the ultra corrosion products are covered on the surface of the zinc-manganese
sonic power increases from 135 W to 180 W, the capacitive reactance phosphate coatings obtained with ultrasonic. It is found that the cor
arc radius of the zinc-manganese phosphate coating actually decreases, rosion degree of the zinc-manganese phosphate coating obtained by
accompanied by a decrease in charge transfer resistance from appropriately increasing the ultrasonic power is reduced compared to
5696 Ω cm2 to 3591 Ω cm2, resulting in poor corrosion resistance. The the zinc-manganese phosphate coating obtained without ultrasonic.
reason is that under the condition of higher ultrasonic power, the The surface of zinc-manganese phosphate coating obtained with
number of cracks on the surface of the zinc-manganese phosphate ultrasonic power of 135 W is relatively compact and is covered with
coating increases, resulting in a decrease in surface density and a de only a small amount of corrosion products after immersing in 3.5 %
crease in the corrosion resistance. sodium chloride solution for 120 h. Based on the above analysis, ap
From Fig. 4(b), it can be seen that the |Z|0.01 Hz of the zinc-man propriately increasing the ultrasonic power is beneficial to form com
ganese phosphate coating obtained without ultrasonic treatment is pact coating with less crystal defects, which are conducive to reducing
higher than that of 16Mn steel, and there is a difference in |Z|0.01 Hz of the degree of corrosion. As shown in Fig. 5(f), the corrosion degree of
the zinc-manganese phosphate coating obtained with and without the zinc-manganese coating obtained with ultrasonic power of 180 W
ultrasonic. As the ultrasonic power increases from 45 W to 135 W, the after immersing in 3.5 % sodium chloride solution for 120 h is sig
|Z|0.01 Hz correspondingly increase from 3605 Ω cm2 to 4625 Ω cm2. nificantly increased compared to the zinc-manganese phosphate
This is because appropriately increasing the ultrasonic power can coating obtained with ultrasonic power of 135 W. This is due to rougher
reduce crystal defects and improve surface density of the zinc-man surface and crystal defects of coating prepared under higher ultrasonic
ganese phosphate coating that contributes directly to the enhance power which decreases the corrosion resistance. Moreover, the corro
ment of corrosion resistance. Compared to 16Mn steel and the zinc- sive medium is prone to penetrate into the interior of the zinc-manga
manganese phosphate coating obtained without ultrasonic, the nese phosphate coating with rougher surface and defects, thereby ac
|Z|0.01 Hz of the zinc-manganese phosphate coating obtained with celerating the corrosion process. The relationship among ultrasonic
ultrasonic power of 135 W has increased by approximately power, surface roughness and corrosion resistance of coating is reported
3015 Ω cm2 and 1590 Ω cm2 respectively. in some published paper as well. Lin et al. study the effect of ultrasonic
However, as the ultrasonic power increases from 135 W to 180 W, on roughness and corrosion resistance of zinc phosphate coating pre
the |Z|0.01 Hz decreases from 4625 Ω cm2 to 2760 Ω cm2. This is due to pared on 20# steel [23]. Yu et al. find that proper ultrasonic power is
the poor surface density of the zinc-manganese phosphate coating beneficial to decrease surface roughness of coatings and improve the
caused by higher ultrasonic power, and the corrosive medium is prone corrosion resistance [24]. Guo and Yao point out that higher ultrasonic
to invade the interior of the zinc-manganese phosphate coating along power during coating preparation will form coatings with rougher
cracks, leading to an accelerated corrosion reaction. surface and poor mechanical performance [25].
a b c
10 μm 10 μm 10 μm
(a) 16Mn steel (b) phosphate coating (without ultrasonic) (c) phosphate coating (45 W)
d e f
10 μm 10 μm 10 μm
(d) phosphate coating (90W) (e) phosphate coating (135W) (f) phosphate coating (180 W)
Fig. 5. Corrosion morphology of different zinc manganese phosphate coatings prepared on the surface of 16Mn steel after immersing in 3.5 % sodium chloride
solution for 120 h (The acceleration voltage is 10 kV with 1200 times magnification and 8 mm working distance).
5
Y. Zhang, X. Chen and H. Tan International Journal of Electrochemical Science 18 (2023) 100274
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formation of Mn-P coatings with significant corrosion resistance on Q235 carbon
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