Tribology International 114 (2017) 257–263

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Effects of nano-SiO2 as water-based lubricant additive on surface qualities MARK

of strips after hot rolling
⁎
Yueyue Bao, Jianlin Sun , Linghui Kong
School of Materials Science and Engineering, University of Science & Technology Beijing, 30 XueYuan Road, Beijing, PR China

A R T I C L E I N F O A BS T RAC T

Keywords: Hot rolling experiments were carried out to study the effect of nano-SiO2 on surface qualities including
SiO2 nanoparticle topography, microstructure and oxide scale of rolled strips. Results show that the surface topography becomes
Topography smooth with the addition of nanoparticles into base lubricant when the concentration of nano-SiO2 is less than
Lubrication 0.5 wt%. Thickness of oxide scale is decreased from 15 µm to 8 µm and the grain size of microstructure on
Rolling
surface is refined simultaneously. Surface qualities are improved due to the better lubrication performances,
which are related to the functions of micro-rolling, polishing and self-repairing of nano-SiO2 on strip surface.

1. Introduction 2. Experiments

With the development of nano-lubricating technology and the deepen-
ing understanding of particularity of functional nano-materials, nanopar-
ticles used as additives show unique physical and chemical properties and
have a broad application prospect in lubrication. Nanoparticles as lubricant
additives such as Cu [1], TiO2 [2,3], Cu/SiO2 [4], SiO2 [5–8], Al2O3 [9], ZnS
[10] and MoS2 [6,11,12] possess outstanding extreme pressure perfor-
mances, excellent anti-wear properties and good lubricating performances.
Padgurskas J et al. [1] studied the tribological properties of Fe, Cu and Co
nanoparticles, experiment results showed that the friction coefficients and
wear of friction pairs significantly reduced with addition of nanoparticles.
Some researchers [5–8] investigated the influence of SiO2 nanoparticles on
the lubricating performance, and results indicated that load carrying
capacity and anti-wear property of the base lubricant can be markedly
improved by adding SiO2 nanoparticles. Liu [10] evaluated the tribological
behavior of ZnS nanoparticles in liquid paraffin, and experiments showed
that nano-ZnS can effectively improve the anti-wear ability and load
carrying capacity of base oil when concentration was 0.1 wt%. At present,
there were a lot of investigations on tribological properties of different
nanoparticles, but the researches about effects of nanoparticles on surface
qualities in the process of lubrication were rarely reported, especially when
nanoparticles applied to hot rolling.
In this study, nano-SiO2 with low cost was selected as additive to
add in water-based lubricant. Hot rolling experiments were carried out
to study the effect of nano-SiO2 added in lubricants on surface qualities
of strips after hot rolling, which provides important reference for the
development of nano-additives.
2.1. Preparation of water-based lubricant containing nano-SiO2
The detailed preparation of nano-SiO2 added in water-based
lubricant is described as follows. Triethanolamine, glycerin and other
lubricant additives were added in deionized water and stirred for
10 min at room temperature using magnetic stirrer to obtain base
lubricant (BL). SiO2 nanoparticles suspended in BL were agitated for
20 min at room temperature, and the water-based lubricant containing
nano-SiO2 could be well dispersed and reserved stably. In order to
avoid the agglomeration of nano-SiO2, nano-lubricant was got in 5 min
before hot rolling experiments. In this work, no dispersants were used
to avoid the effects of the dispersants on the results. SiO2 nanoparticles
were commercially provided by chemical reagent supplier Shanghai,
China. Micrograph of SiO2 nanoparticles was investigated by TEM
(JEM-2010) and shown in Fig. 1. It shows that SiO2 nanoparticles
represent a spherical shape and have a mean diameter of 30 nm.
2.2. Hot rolling experiments
Different lubricating conditions were used to study the effect of
nano-SiO2 on surface qualities of strips after hot rolling, including BL
with the concentration of nano-SiO2 was 0, 0.1 wt%, 0.3 wt% and
0.5 wt% respectively. The concentration values were referred to the
results that appropriate concentration of nanoparticles added in
lubricants was in the range of 0.1–1 wt% [13–15]. Experiments of
hot rolling were conducted on the F350mm four-high mill and the
material was ASTM 1045 steel (the silicon content is between 0.17%

⁎
Corresponding author.
E-mail addresses: 2897104376@qq.com (Y. Bao), sjl@ustb.edu.cn (J. Sun), 358788353@qq.com (L. Kong).

http://dx.doi.org/10.1016/j.triboint.2017.04.026
Received 22 January 2017; Received in revised form 13 April 2017; Accepted 17 April 2017
Available online 18 April 2017
0301-679X/ © 2017 Elsevier Ltd. All rights reserved.
Y. Bao et al. Tribology International 114 (2017) 257–263

surface roughness. To ensure the accuracy of the data, each group of

the samples was measured for 12 times and the determined value was
obtained by averaging 12 measurements. After the process of mechan-
ical polishing, the surface was etched for 3 s with nitric acid alcohol
which was a mixture of 96% alcohol and 4% nitric acid before
microstructure analysis. The thicknesses of rolled strips after rolling
were measured by using a micrometer and each final result was
obtained by averaging 10 measurements. Brinell hardness of the
eroded samples was conducted on a hardness tester; the applied load
and holding time was 100 kg and 60 s. Only four data were measured
on each sample due to the small size. While prior to the surface oxide
scale analysis, samples were made into 20 mm in diameter and 20 mm
in thickness cylinder with phenolic plastic, and one cross section of the
samples was exposed in air and was milled and polished to Ra <
0.1 µm.
Surface topography and oxide scale of strips were analyzed with SEM
(ZEISS-EVO18) to research the effect of nano-SiO2 on the anti-wear
property and oxidation resistance respectively. 3-D topographies and
Fig. 1. TEM micrograph of nano-SiO2.
surface roughness of the strips were observed on CLSM (Olympus LEXT
OLS4000), besides the microstructures of strip surface were conducted on
an Optical Microscope (ZEISS AX10) to explore the influence of nano-
SiO2 on structure properties of strip surfaces. For the purpose of the
operation mechanism of nano-SiO2, EDS (ZEISS EVO18) was conducted
to analysis elements on strips surface and XPS (ESCALAB 250Xi) was
performed to determine the chemical states of typical elements on strips
surface.

3. Results and discussion

3.1. Effect of nano-SiO2 on surface topography

Surface topographies of the rolled strips under different lubricating

conditions are shown in Fig. 3. Surface of rolled strip shows sign of
intensive pits and cracks when lubricated with BL. The appearance of
pits is on account of oxide scales and other hard materials press into
Fig. 2. The sketch of hot rolling.
the strips and then fall off from surface. And cracks are formed by the
rupture of oxide scales, which are with poor ductility and under
horizontal or vertical expansion stress in the process of rolling. There
Table 1
Conditions of rolling experiments. are also dense scratches, which were due to the scratching of oxide
scales adhered on the rolls. Furthermore, the surface is quite unsmooth
Parameter Value with a lot of salient. With the increase concentration of nanoparticles,
pits and cracks as well as salient are gradually reduce compared with
Initial thickness H /mm 30
Heat temperature /°C 1000 that lubricated with BL. In addition, surface becomes so smooth that
Holding time t /h 1.5 there are few salients could be observed. Furthermore, there is no
Start rolling temperature /°C 950 obvious change of surface lubricated with 0.3 wt% and 0.5 wt% nano-
Finish temperature /°C 750 SiO2 except for the reduction of oxide scales and cracks. It indicates
The speed of rolling v / (m s −1) 2.0
that surface defects of rolled strips can be significantly reduced and the
surface topography can be improved obviously by adding nanoparti-
−0.37 wt%). The sketch of hot rolling is shown in Fig. 2. A special cles. The reason why oxide scales reduced will be explained in Section
laboratorial lubrication device (pressure of 0. 15 MPa, flow of 4.5 L/ 3.3.
min, temperature of 60 °C) was used in lubrication of the work roll, and In order to conduct a comprehensive study about the effects of
mechanical descaling of strips was conducted before rolling and the nanoparticles on the surface topography, 3-D topography of strip
strips were cooling in the air before being used in other tests. The detail surface was measured in this work. Fig. 4 exhibits 3-D topographies
conditions of rolling experiments are shown in Table 1. Rolling gaps of the rolled strips under different lubricating conditions. The peaks on
designed for each rolling pass were 22 mm, 16 mm, 10 mm, 6 mm and strip surface are reduced and the surface becomes more and more
4 mm respectively. smooth when the concentration of nanoparticles is less than 0.5 wt%.
However, the surface roughness increases slightly with more scratches
when content of nanoparticle is 0.5 wt%. The date in the bottom left
2.3. Sample preparation and characterization methods corner of figures are liner roughness of samples, which corresponding
to the change rule of surface topographies. The results of these two
For the test of the surface quality of samples after hot rolling, five experiments manifest that the addition of SiO2 nanoparticles makes the
discs with the sizes of 10 mm*10 mm were cut from the center of the surface topography smooth when the content of nano-SiO2 is no more
strips and the distance between each block was 10 mm. The samples than 0.3 wt%. And further addition of nanoparticles would not have
can be directly used for surface morphology and roughness analysis noticeable influence on surface topography. The reasons why surface
after rinsing with petroleum ether, and the linear roughness which topography improved by adding nano-SiO2 will be detailed discussed in
perpendicular to the rolling direction was measured to characterize the Section 3.4.

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Fig. 3. Surface topography of the rolled strips under different lubricating conditions: (a) BL, (b) BL +0.1 wt% SiO2, (c) BL +0.3 wt% SiO2, (d) BL +0.5 wt% SiO2.

3.2. Effect of nano-SiO2 on microstructure
The phases of strip surfaces after rolling under different lubricating
conditions are shown in Fig. 5. The microstructures of strip surfaces
after rolling are pearlite and ferrite, while matrix phase is pearlite and
second phase in grain boundaries is ferrite. It can be seen from
Fig. 4(a) that the microstructures of strip surface are pearlite and a
few ferrite when lubricated with BL. After adding 0.1 wt% SiO2
nanoparticles, the size of pearlite significantly decreases and the
content of ferrite increases at the same time. When the addition of

Fig. 4. 3-D topographies of the rolled strips under different lubricating conditions: (a) BL, (b) BL +0.1 wt% SiO2, (c) BL +0.3 wt% SiO2, (d) BL +0.5 wt% SiO2.

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Fig. 5. The microstructures of rolled strips under different lubricating conditions: (a) BL, (b) BL +0.1 wt% SiO2, (c) BL +0.3 wt% SiO2, (d) BL +0.5 wt% SiO2.

nanoparticles are 0.3 wt% and 0.5 wt%, the microstructures have no 4.5 75.0

obvious change compared with that lubricated with 0.1 wt% SiO2 Thickness
nanoparticles. It indicates that the addition of nano-SiO2 makes grains HRB
of strip surface refined and the contents of ferrite increase. 74.5
Factors that might have contribute to the decrease of grain size and 4.4
Thickness/mm

the increase content of ferrite shall be discussed. The first reason might
be the faster cooling rate of nano-lubricant. The increasing of cooling

HRB
74.0
rate contributes to the formation of crystal nucleus, which contributes
to the refinement of grain size and helps accelerate the transformation
4.3
of ferrite. While cooling rate depends on the thermal conductivity of the
liquid. Choi and Eastman et al. [16] tested the coefficients of thermal 73.5

conductivities of Al2O3-water, SiO2-water, TiO2-water and other nano-

liquids. The experiment results showed that the thermal conductivity of
nano-liquid increased by more than 60% than that of water when the 4.2 73.0
volume fraction of nanoparticles was less than 5%. Many researchers BL BL+0.1wt.% SiO2 BL+0.3wt.%SiO2 BL+0.5wt.%SiO2

have used different nanoparticles to the preparation of nanometer fluid Lubricating conditions
[17–19] and obtained similar results: the thermal conductivity of the
Fig. 6. The thickness and hardness of rolled strips under different lubricating condi-
solution will be greatly improved by adding a small amount of
tions.
nanoparticles. But experimental data were lacking consistency and
the reason why thermal conductivity of liquids increase by adding
are all the same. So it's helpful to reduce the friction coefficients of the
nanoparticles was not unified [20,21]. Besides, in our work, the dosage
lubricant by adding nanoparticles. Conclusion can be drawn that the
of lubricating conditions sprayed on the roll was small and the contact
addition of nanoparticles would result in decrease of the friction
time of roll and strips was short, which made it not sure whether it is
coefficients, which makes the deformation increase.
thermal conductivity has a great influence on microstructure.
Hardness of microstructure is direct related to grain size, therefore
Another reason may be the effect of plastic deformation. In the process
the hardness of strip surface after rolling under different lubricating
of preheating, Fe has transformed into austenite completely after steel
conditions is plotted in Fig. 6. Surface hardness increases gradually with
plate being heated for 1.5 h at 1000 °С. Plastic deformation is helpful to
the addition of nanoparticles, which is consistent with the microstruc-
the diffusion of iron and carbon and nucleation of grains, which
ture of strips, namely the smaller the grain size is, the higher surface
contributes to the decrease of the grain size. The thickness after rolling
hardness will be.
and hardness of strips after rolling under different lubricating conditions
are plotted in Fig. 6. The thickness of strip lubricated with BL decreases
with the addition of nanoparticles. When the content of nano-SiO2 is 3.3. Effect of nano-SiO2 on oxide scale
0.3 wt%, the thickness of strip reaches minimum value. The higher
content of nanoparticles is, the bigger plastic deformation will be. In Fig. 7 represents the oxide scales of rolled strips under different
addition, when content of nanoparticle is 0.3 wt%, decrease rate of lubricating conditions. As the processes of hot rolling are all the same,
thickness can reach 5%. According to Stone formula, reduction of strip difference in oxide scales of strips is only relates to the different
is only relates to friction coefficients when other experimental conditions lubricating conditions. As is shown in Fig. 7, the thickness of oxide

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Fig. 7. The oxide scales of rolled strips under different lubricating conditions: (a) BL, (b) BL +0.1 wt% SiO2, (c) BL +0.3 wt% SiO2, (d) BL +0.5 wt% SiO2.

scale with loosen structure is about 15 µm, and there are many voids in 50

oxide scales, in addition, the interface combines oxide scale with the 45

matrix is extremely unsmooth when lubricated with BL. While oxide 40

scale becomes compact and thin, and interface become more smoother 35
Heat Flow /mW

when adding SiO2 nanoparticles. But there are almost nothing change 30
of oxide scale when the concentration of nano-SiO2 reaches 0.5 wt%. 25
Moreover, the thickness of oxide scale decreases to 8 µm and there are 20
almost no voids in oxide scale when adding 0.3 wt% SiO2 nanoparti- 15
cles. 10
Researches showed that the thickness of oxide scale closely related to 5
deformation of strips, which decreased with the increase of deformation 0
[22]. Seen from Fig. 6, the deformation of strips increases when adding -5
SiO2 nanoparticles and minimum thickness of strips is 4.26 mm when 100 200 300 400 500 600 700 800 900 1000

the concentration of nano-SiO2 is 0.3 wt%. While friction coefficients Temperature/°C

have direct influence on deformation of strips, namely deformation
increases with the decrease of friction coefficients. Therefore, the
addition of nano-SiO2 reduces thickness of oxide scale through decreas-
ing friction coefficients.
3.4. Inquiry of lubrication mechanism
In order to research the lubricating mechanism of SiO2 nanopar-
ticles, differential thermal analysis of SiO2 nanoparticles was tested.
Fig. 8 shows differential thermal analysis curve of SiO2 nanoparticles.
It illustrates that the melting point of SiO2 nanoparticles is about
700 °C. The temperature of strip is 1000 °C at first rolling pass, which
gradually decreases with the increases of rolling pass. Contact time of
strip and roll is only a few seconds because of high rolling speed.
Therefore, there is no time for nanoparticles to melt, so nanoparticles
keep solid form in the rolling process.
Lubricating mechanism of SiO2 nanoparticles as additive is not
unified. Rolling friction mechanism, thin film lubrication mechanism,
boundary lubrication layers and so on [23] have been proposed in the
past few years. However, the lubricating mechanism of nanoparticles is
not a single one, it's a synergy of above mechanisms. Fig. 9 is the EDS
spectra of strip surface lubricated with 0.5 wt% SiO2 nano-lubricant. As
is shown in Fig. 9, there is Si element on strip surface defects, which
Fig. 8. Differential thermal curve of SiO2 nanoparticles.
illustrates that nanoparticles deposit on surface. XPS of strip surface
under 0.5 wt% SiO2 nano-lubricant were analyzed to further study the
lubricating mechanism of SiO2 nanoparticles. The typical chemical
state of elements analysis results are shown in Fig. 10. According to the
NIST Standard Reference Data base 20 (version 4.1), a weak Si2p peak
emerges at 103.72 eV [24], which associates with the O1s at 532.57 eV
[25] well corresponding to the Si2p and O1s of SiO2. The band of O1s
at 530.57 could be identified as Fe2O3 [26]. Moreover, two Fe2p peaks
emerge at 710.47 eV and 724.32 eV attribute to Fe2p of Fe3O4 [27] and
Fe2O3 [28] respectively. It is indicate that there is no reaction of SiO2
nanoparticles and the lubricating effect is only by physical effect.
The physical model of SiO2 nanoparticles as lubricant additive in
rolling is described in Fig. 11. Under the contact load, based liquid and
nanoparticles are dragged into the friction pairs, forming a thin
physical lubricating film, which possesses a lot of important functions,
such as bearing the load and avoiding direct contact of the friction pairs
[29,30]. For A, nanoparticles grind the peaks under the effect of high
pressure and speed of roll, which make the peaks shorter, thus have a
polishing effect on strip surfaces. For B, nanoparticles play a self-
repairing role on worn surface by depositing into depressions. As for C,

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Fig. 9. EDS spectra of strip surface lubricated with 0.5 wt% SiO2 nano-lubricant.

a part of sliding friction is turned into rolling friction attributes to

spherical shape of nano-SiO2, thus reducing the friction coefficients,
and wear of surface decreased simultaneously. Addition of SiO2
nanoparticles plays a role in bearing the load and avoiding the contact
of the friction pairs, which reduces the adherence of oxide scales on
rolls, so as to reduce the amount of pits and scratch. In addition, rolling
effects and self- repairing mechanism of nano-SiO2 also contributes to
the reduction of pits and scratch, and salient flattened due to the
polishing effect of SiO2 nanoparticles. All of the effects of nanoparticles
improve the surface quality of rolled strips, thereby raising the anti-
wear performance of BL. However, agglomeration of SiO2 nanoparti-
cles becomes obvious, which on account of the high surface energy and
make wear and friction coefficients slightly increase when the concen- Fig. 11. Physical model of nanoparticles as additive and the large view of A, B and C.
tration of nano-SiO2 was 0.5 wt%. Decreasing of surface roughness and

1200

Si2p 8000
O1s
532.57
1100 6000 530.57
103.72
Intensity

Intensity

4000

1000

2000

900 0
98 99 100 101 102 103 104 105 106 107 108 526 528 530 532 534 536 538 540

Binding Energy/ev Binding Energy/ev

7000

Fe2p 710.47
724.32
6000
Intensity

5000

4000

3000

2000
705 710 715 720 725 730

Binding Energy/ev
Fig. 10. XPS spectra of Si 2p, O 1 s and Fe 2p on the wear surface lubricated with 0.3 wt% SiO2 nanoparticles.

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rolling effect of nano-SiO2 contribute to the decline of friction
coefficients, which increase deformation of strips. Then grain of surface
refined and surface hardness increases because of increase of deforma-
tion. As for oxide scale, the increase deformation of strips also
contributes to the reduction of oxide scale thickness. Furthermore,
the deposition of SiO2 nanoparticles hinders the contact of surface with
air, which makes the oxide scale thickness become thinner, and oxide
scale becomes denser due to the deposition of SiO2 nanoparticles in
surface defects.
4. Conclusions
Based on the analysis of the surface qualities of strips lubricated
with different lubricating conditions, the following conclusions could
be drawn.
1. The surface topography of strips lubricated with BL has been
obviously improved by adding nano-SiO2, when the concentration
is less than 0.5 wt%.
2. By adding nano-SiO2 in the base lubricant, the sizes of grains on the
surface of strip are refined and the amount of pearlite is increased
simultaneously. In addition, the oxide scale becomes thinner and
denser with a maximum reduction of 7 µm of the thickness when the
concentration of nano-SiO2 is 0.3 wt%.
3. The results that SiO2 nanoparticles enhance the surface qualities of
strips can be explained to the improvement of the lubrication
performance during the rolling process, which is related to the
functions of micro-rolling, polishing and self-repairing of nano-SiO2.
Acknowledgement
This work was supported by the National Natural Science Foundation
of China (Grant No. 51474025).
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