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Procedia Engineering00
Procedia Engineering00 (2017)
(2017) 000–000
000–000
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ScienceDirect
Procedia Engineering 207 (2017) 2227–2232

International Conference on the Technology of Plasticity, ICTP 2017, 17-22 September 2017,
Cambridge, United Kingdom

Effects of lubricants on the rolling performances of cold rolled

copper strips
Xudong Yan, Jianlin Sun*, Sang Xiong
School of
School of Materials
Materials Science
Science and
and Engineering,
Engineering, University
University of
of Science
Science and
and Technology
Technology Beijing,
Beijing, 30
30 Xueyuan
Xueyuan Road,
Road, Beijing,
Beijing, 100083,
100083, P.R.
P.R. China
China

Abstract
Abstract

Two parameters
Two parameters inin rolling
rolling process,
process, the the forward
forward slip
slip value
value (S
(Shh)) and
and thethe minimum
minimum rolling
rolling gauge
gauge (h
(hmin
min)) were
were tested
tested using
using aa 4-high
4-high
rolling mill in order to investigate the rolling performances of cold rolled copper strips under different lubricating
rolling mill in order to investigate the rolling performances of cold rolled copper strips under different lubricating conditions viz, conditions viz,
lubrication with
lubrication with (i)
(i) base
base oil,
oil, (ii)
(ii) base
base oiloil with
with 0.5wt.%
0.5wt.% oiliness,
oiliness, (iii)
(iii) base
base oil
oil with
with 0.5wt.%
0.5wt.% dialkyldithiophosphateester(DDE)
dialkyldithiophosphateester(DDE) and and
(iv) base
(iv) base oil
oil with
with 0.25wt.%
0.25wt.% DDE DDE and and 0.25wt.%
0.25wt.% molybdenum
molybdenum dialkyldithiophosphate
dialkyldithiophosphate (MoDDP).
(MoDDP). The The surface
surface roughness
roughness of of rolled
rolled
copper strips
copper strips was
was measured
measured by by aa laser
laser scanning
scanning confocal
confocal microscope.
microscope. The The surface
surface morphologies
morphologies of of copper
copper strips
strips were
were observed
observed
by aa scanning
by scanning electron
electron microscopy
microscopy (SEM) (SEM) andand the
the compositions
compositions of of the
the surface
surface residues
residues were
were analyzed
analyzed with
with an
an energy
energy dispersive
dispersive
spectrometer (EDS).
spectrometer (EDS). Results
Results showed
showed friction
friction coefficients,
coefficients, which
which were were calculated
calculated byby SShh with
with different
different lubricants
lubricants ranged
ranged from
from
0.067-0.302. The
0.067-0.302. The surface
surface topography
topography of of copper
copper strips
strips showed
showed smoothsmooth and and the
the plowing
plowing wearwear was
was finer.
finer. Meanwhile,
Meanwhile, whenwhen thethe
lubricant was
lubricant was base
base oil
oil with
with 0.25wt.%
0.25wt.% DDE DDE andand 0.25wt.%
0.25wt.% MoDDP,
MoDDP, the the hhmin of copper
min of copper reached
reached 19μm,
19μm, aa value
value satisfied
satisfied the
the copper
copper
foil conduction.
foil conduction. However,
However, with with the
the addition
addition ofof EP
EP additives,
additives, the
the topographies
topographies showed
showed somesome grind
grind pits
pits at
at local
local region.
region. Indicating
Indicating
that EP
that EP additives
additives containing
containing P, P, S,
S, Mo
Mo moieties
moieties possess
possess aa better
better thickness-reducing
thickness-reducing performance,
performance, butbut cause
cause corrosion
corrosion atat the
the same
same
time.
time.
© 2017
© 2017 The
The Authors.
Authors. Published
Published by by Elsevier
Elsevier Ltd.
Ltd.
© 2017 The Authors.
Peer-review under Published by
responsibility of Elsevier
the Ltd.
scientific committee of the International Conference on the Technology
Peer-review under
Peer-review under responsibility
responsibility of of the scientific committee of the International Conference on the Technology of Plasticity.
of Plasticity..
Keywords:Cold rolled
Keywords:Cold rolled copper
copper strips;
strips; Forward
Forward slip
slip value;
value; Minimum
Minimum rolling
rolling gauge;
gauge; Mixed
Mixed film
film friction
friction

** Corresponding
Corresponding author.
author. Tel.:
Tel.: +86-010-62333768
+86-010-62333768
E-mail address:
E-mail address: sjl@ustb.edu.cn
sjl@ustb.edu.cn

1877-7058 ©
1877-7058 © 2017
2017 The
The Authors.
Authors. Published
Published by
by Elsevier
Elsevier Ltd.
Ltd.
Peer-review under
Peer-review under responsibility of the scientific committee of the International Conference on the Technology of
responsibility of
Plasticity..

1877-7058 © 2017 The Authors. Published by Elsevier Ltd.

Peer-review under responsibility of the scientific committee of the International Conference on the Technology of Plasticity.
10.1016/j.proeng.2017.10.986
2228 Xudong Yan et al. / Procedia Engineering 207 (2017) 2227–2232
2 Xudong Yan et al. / Procedia Engineering00 (2017) 000–000

1. Introduction

Rolled copper foil is widely used in manufacture of print circuits due to its excellent electrical conductivity,
thermal conductivity, reliability and chemical resistance [1, 2]. During the cold rolling process, since the rollers and
the work piece are in close contact, friction and wear will inevitably occur and increase the energy loss [3, 4].
Technological lubrication is one of the key factors to improve the technology for rolling of copper foil. Suitable
lubricants possess excellent extreme-pressure properties, cooling performances and anti-wear properties so that the
fiction coefficient, rolling pressure, and power consumption are significantly reduced.
Researchers have shown more interest in lubricants, with which the thin and cheap rolled copper foils were
fabricating. Huang [5] applied physical and chemical experiments on copper foil with a developed oil, the results
showed that the developed oil has a good performance of oil film bearing capacity and oxidation resistance. Wen [6]
has found the coefficient of friction (COF) was reduced with the addition of nano-TiO2 particles into the 1.0%
(mass %, oil concentration) O/W lubricant. Huh [7] has analyzed the microstructures of copper with and without
lubricants after cold rolling and founded the copper samples without lubricants showed a very inhomogeneous as-
deformed microstructure consisting of rhombus-like parallelograms surrounded by shear bands while a better
microstructure was obtained when lubricant was used.
Although numerous studies about the tribological properties of lubricant or its impacts on copper structure have
been done, the performances of lubricants on cold rolling, the friction conditions, as well the surface qualities of
cold rolled copper are yet to be determined. In this paper, in order to investigate the rolling performances of cold
rolled copper strips under different lubricating conditions viz, lubrication with (i) base oil, (ii) base oil with 0.5wt.%
oiliness, (iii) base oil with 0.5wt.% dialkyldithiophosphateester (DDE) and (iv) base oil with 0.25wt.% DDE and
0.25wt.% molybdenum dialkyldithiophosphate (MoDDP), two parameters in rolling process, the forward slip value
(Sh) and the minimum rolling gauge (hmin) were tested using a 4-high rolling mill. The influences of the roughness
and oil film thickness on friction conditions were also addressed. Further, the surface topographies of rolled copper
foil were obtained.
Nomenclature

Sh the forward slip

hmin the minimal rolling gauge
L the length of two consecutive points
Ln the length after rolling
μ the mean friction coefficient
△h reduction in height of the rolled strip
R the radius of roller
h the rolling gauge
hoilfilm the oil film thickness
Ra the surface roughness
λ the ratio of hoilfilm and Ra

2. Experimental materials and methods

Acetone, petroleum ether were used for cleaning rolled piece before each test. The specific physiochemical
properties of Mineral base oil, D130 are given in Table 1 (in ASTM). 1-Dodecanol and Butyl stearate were utilized
as oiliness additives with the proportion of 2:3. Dialkyldithiophosphate ester (DDE) and molybdenum
dialkyldithiophosphate (MoDDP) were the compositions of EP additives. For the tests, lubricants were prepared by
adding only oiliness additives, only DDE or mixture DDE and MoDDP as composite EP additives to the bass oil.
The lubricants were consisted of 0.5wt.% additives and 99.5wt.% base oil.
 Xudong
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et al.et/al. / Procedia
Procedia Engineering
Engineering 207 (2017)
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Table. 1. Physiochemical properties of D130

Main characteristics Parameter

Density(25℃), g/ml 0.824
Dynamic viscosity(25℃), mm2/s 6.12
Flash point(open), ℃ 140
Boiling range, ℃ 279-313
The experimental materials were C11000 (with a purity of 99.9%) copper strips that prepared with 0.5mm in
thickness, 50mm in width before cold rolling. A 4-high rolling mill of Φ95/200mm×200mm with a velocity of
60r/min and a rolling power of 35kW was used to evaluate the rolling performances under different lubricating
conditions. The reduction ratios of each pass are restricted by 20% and the rolled strips were collected, measured
and compared after each pass. After the roller was in the work roll edge contact, the copper strips were rolled for
another 4 passes to get the minimal rolling gauges. Another parameter of rolling, Sh was obtained after the number 4
pass of each rolling experiments. The principle diagram of the forward slip experiments was shown in Fig.3. The
mean friction coefficient of work pieces under different lubricating conditions could also be deduced according to
the equations as below.

Fig. 1. The principle diagram of the forward slip experiments

Ln  L
Sh 100% (1)
L
h
μ R (2)
S h
2(1-2 h )
h
The rolled pieces used in the experiments were analyzed with respect to surface properties and wear
characteristics using various analytical tools. The surface roughness of the rolled pieces was measured with a
German model LEXT OLS4000 laser confocal microscope. The surface topographies of copper foils were observed
by a scanning electron microscopy (SEM) and the compositions of the surface residues were analyzed with an
energy dispersive spectrometer (EDS).

3. Results and discussion

3.1. Rolling performances

The rolling forces and the rolling gauges were measured after each passes. The result was shown in Fig.2 (a) and
Fig.2 (b).
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Fig. 2. Evolutions of (a) rolling forces and (b) rolling gauges via rolling pass under different lubrications. (25 ℃, 35 KW, 60 rpm)
It can be seen from Fig.2 (a), due to the effect of work hardening mechanism, the rolling forces rose at the first 5
rolling passes while dropped after the roller was in the work roll edge contact. When lubricants were introduced, the
rolling forces obviously reduced at each pass. It is obvious that a lowest rolling force was obtained when the
lubricant was D130 + 0.25wt.% DDE + 0.25wt.% MoDDP.
Besides rolling forces, the minimum rolling gauges (Fig.2 (b)) showed that base oil containing EP additives had
better rolling performances. The minimum rolling gauges reduced and satisfied the copper foil production.
Especially for the lubricants was D130 + 0.25wt.% DDE + 0.25wt.% MoDDP, it obtained the lowest minimum
rolling gauge with a value of 0.19μm. These results indicate that composite EP additives generate a synergistic
effect on rolling efficiency improvement.

3.2. Friction conditions

The relative parameters of the forward slip experiments were listed in Table. 2. When using lubricants, the
friction conditions of copper strips changed from dry lubrication to boundary lubrication [8]. Especially with the EP
additives containing only DDE or mixture DDE and MoDDP, the mean friction coefficient reached a properly low
value of 0.089 and 0.067, respectively. It can be concluded that a stable tribo-film formed with the addition of EP
additives and changed the friction conditions.

Table. 2. Parameters of the forward slip experiments

Lubricating conditions △h(mm) Sh(mm) μ hoilfilm(10-3mm) Ra(10-3mm) λ

No lubrication 0.095 0.050 0.88 - 0.635 -
Base oil(D130) 0.092 0.068 0.302 0.013 0.325 ＜0.1
D130+oiliness 0.090 0.100 0.187 0.031 0.375 ＜0.1
D130+0.5 wt% DDE 0.088 0.114 0.089 0.287 0.253 ≈1
D130+0.25 wt% DDE +0.25 wt% MoDDP 0.088 0.127 0.067 0.265 0.275 ≈1
According to Th. Mang’s theory [9], λ reflects the ratio of film thickness and surface roughness can be used to
further demonstrate the friction conditions with different lubrication. An oil drop method was applied to investigate
the oil film thickness in lubricant rolling. The tests involved dropping a known quality of oil on the rolled piece
surface before rolling, measuring the coverage area with a mark-ups paper after rolling. The drop volume divided by
the surface area of the mark gives the final thickness of oil film thickness hoilfilm. Combining with the value of
surface roughness (Ra), the value of λ can be obtained.
Obviously, when the copper were lubricated with base oil or D130 + 0.5 wt.% oiliness, the value of λ were less
than 1, showed the boundary lubrication of these two conditions. Conversely, for the conditions of lubricants with
 Xudong Yan et al. / Procedia Engineering 207 (2017) 2227–2232 2231
Xudong Yan et al. / Procedia Engineering 00 (2017) 000–000 5

EP additives, the value of λ were approximate to 1, demonstrating a mixed-film lubrication, which reduced the
friction and changed the surface qualities at the same time.

3.3. Surface topographies

The 3D topographies of rolled copper surface showed various with different lubrication. When only base oil was
used (Fig.3(a)), there was noticeable adhesion with deep rolled trace on the copper surface. Simultaneously cracks
and peeling existed and formed a relatively coarse topography. Oiliness added (Fig.3(b)) improved the surface
glossiness and the topography was clean. Furrows and plowing were the main forms of wear on copper surface.
Importantly, when only DDE was introduced (Fig.3(c)), the plowing was finer and the surface roughness
significantly reduced. Meanwhile some grind pits were generated around the rolled traces. When the strips were
lubricated with D130+ 0.25 wt.% DDE+ 0.25 wt.% MoDDP (Fig.3(d)). The pits and surface roughness increased,
which could attribute to the corrosion caused by those composite EP additives.

Fig.3. The 3D topographies of rolled copper surface under different lubricating conditions: (a) base oil, (b) D130+0.5wt.% oiliness
(c) D130+0.5wt.% DDE and (d) D130+ 0.25 wt.% DDE+ 0.25 wt.% MoDDP

To further investigate the composition of the residues on copper surface, the topography of copper lubricated
with D130+ 0.25 wt.% DDE+ 0.25 wt.% MoDDP was enlarged to 1000 times with SEM and an EDS analysis had
been done. As it can be seen in Fig.4, 1# and 2# represented the area of rolled traces and grind pits, respectively.
Cleary there were grind pits existed around the fine plowing. 1# showed 92.17% Cu and an extremely low amount
of C (7.83 %) on the rolled trace, while only 83.08% of Cu was presented on 2#, along with 7.83%, 4.78%, 2.45%,
1.86% of O, Mo, S, P elements, respectively. These results attribute to Mo, P, S moieties generate oxidation
corrosion pits. Indicating that EP additives process the ability to finer rolled traces, but could also lead to corrode the
surface at local region.
6 Xudong Yan et al. / Procedia Engineering00 (2017) 000–000
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Fig.4. SEM images and EDS analysis of copper surface lubricated with D130+ 0.25 wt.% DDE+ 0.25 wt.% MoDDP

4. Conclusions

With the addition of oiliness additives and EP additives into base oil, the rolling forces obviously reduced. A 19
μm copper foil was obtained when the copper was lubricated with D130+ 0.25 wt.% DDE+ 0.25 wt.% MODDP.
Lubricants changed the rolling friction conditions from dry lubrication to boundary lubrication. Especially for the
condition that lubricated with base oil with EP additives, the value of oil film thickness was approximate to the
surface roughness, indicating a stable tribo-film formed on copper surface.
EP additives made rolled traces finer, and oxidation corrosion pits generated on the surface, which caused by Mo,
P, S moieties in additives.

Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (Grant No. 51474025).

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