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Rolling oils are formulated with many components like lubricity agents, synthetic esters,
anti-wear additive, extreme pressure additive, emulsifier, anti oxidants, anti-carbon
additive, anti-corrosion additive, biocide, etc. The oils are also designed to have varying
properties including some special properties like ion rejection properties, tramp oil
rejection properties, hydrolytic stability, thermal stability, detergency, etc. There is
usually more than one choice for each additive in the oil. Thus formulation of candidate
oil for a given mill is not simple. Oil formulators select the types and doses of these
additives based on rolling conditions like type of material to be rolled, geometry of roll
bite (draft, reduction, roll diameter), mode of application (direct or re-circulation), mill
speed, surface finish to be given to the strip, possible chemical reactions with the strip,
further processing of the rolled strips, make-up water type, type and level of
contaminants, etc.
Selection of candidate rolling oil based on its performance can be divided in four groups:
(a) Evaluation of physico-chemical properties of the oil,
(b) Evaluation of tribological characteristics of the oil at laboratory rigs,
(c) Evaluation of rolling performance of the oil at laboratory mill, and
(d) Evaluation of actual performance of the oil at industrial mill.
Based on the laboratory performance of the candidate oil, its formulation can be
optimised. The optimised formulation can be re-evaluated in the laboratory and if found
suitable, it may be recommended for field trial at the industrial mill.
Properties Value
Kinematic viscosity, cSt at 40 oC 30-60
Saponification value, mg KOH/g 90-200
Free fatty acid, mg KOH/g (% Oleic) 5-20
Iodine value, g I2/g 20-55
pH in distilled/demineralised water 5-8
Emulsion stability index (ESI) 0.80-0.95
Mean oil particle size, m 2-12
Ash content, weight % 0.00-0.10
Carbon residue (CCR), weight % 0.10-0.50
Pour point, oC 0-20
Flash point, oC, (COC) 200-250
(b) Saponification Value: Sap value may be determined by method of titration as per
ASTM D94 standard. It denotes the weight of potassium hydroxide, expressed in
milligrams, required to saponify one gram of the oil or fat to produce soap and glycerine.
Higher the sap value is preferred for better lubricity, however, it may adversely affect
cleanliness performance of the oil.
(c) Free Fatty Acid (FFA) Value: The organic acidity of an oil or fat is usually
expressed in either of two ways: (a) As weight % of free fatty acid present (molecular
weight of which is arbitrarily assumed to be 282, 256 or 200 corresponding to oleic,
palmitic or lauric acid), and (b) As the total acid number. The total acid value is measured
by the method of titration where it is the number of milligrams of potassium hydroxide
required to neutralise the acidity of one gram of the oil or fat. The free fatty acid value of
the oil is approximately taken as half the value of total acid number.
Flat Rolling Lubrication
(d) Iodine Value: Iodine value gives the degree of unsaturation of fatty materials and is
measured by titration method involving reaction with pyridine bromide solution.
In all the methods, a heated sample of the oil is mixed with a specified quantity of water
in a specially designed container to make an emulsion. Mixing rate/speed, time and
temperature vary from experiment to experiment. The emulsion is then sampled at
specified times and then poured into specified flasks and treated with specified acid split
solution. Each flask is then placed in either an oven or boiling water bath in order to
promote oil separation. The volume of separated oil can then be read off using the scale
on the flask. Finally plotting oil content against the time generates a demulsification
curve. An emulsion stability index (ESI) is also calculated in either of the following two
ways:
Oil2 OilBottom
ESI Or, ESI
Oil1 OilTop
Where, Oil1 is initial oil concentration and Oil2 is oil concentration after a specified time.
Similarly, OilTop and OilBottom are oil concentrations in respectively top and bottom layers
of emulsion after a specified time.
The effect of emulsion age, contamination and/or shear rate on the emulsification
characteristics or oil particle size can be studied by re-circulating the emulsion in the
specified rig. Different rigs are available for study of emulsification characteristics of the
Chapter V Lubricant Management
oil. Some of them are: Ultraturrax Mixer, Tempunit, Braun Mixer, Oil Breakout Set-up,
etc.
(f) Oil Particle Size: There are some dedicated equipments for measuring oil particle size
in emulsions. For example: Coulter laser particle size analyser, Malvern particle size
analyser, etc. Normal optical microscope can also be used to measure oil particle size on
a slide of emulsion. Using sophisticated equipment, study can be made on the
dependency of oil particle size on various parameters like agitation or shear stress,
temperature, time, etc. as well as type and dose of additives.
Shear stability of the oil is measured in terms of change in oil particle size with applied
shear force. A stable rolling oil exhibits practically no change in its particle size with
application of shear force. On the other hand, unstable oil exhibits maximum change
(reduction) in particle size under such condition. The optimum stability may be designed
in metastable oil.
(f) Ash Content: It is measured by burning/evaporating the oil under controlled condition
furnace.
(g) Carbon Residue: There are few test methods in which level of carbon residue is
measured after breaking the oil under controlled condition. Condradson Carbon Residue
(CCR) Test is one such methods, in which carbon-forming tendency of rolling oil is
studied under specified pyrolysis condition.
Evaluation of Lubricity: There are various test rigs available today for evaluating
lubricity of the rolling oils. Some of these rigs are Soda Pendulum Lubricity Test Rig,
SRV Test Rig, Falex Pin and V Block machine, LFW-1 Test Rig, and Plint Tribometer.
Details of contact configuration of these test rigs have been given in Table 5.2. In these
tests, lubricity of oil is measured in terms of friction coefficient, critical load/torque, and
wear rate/scar. Some of typical results achieved with successful rolling oils are shown in
Table 5.3.
In all the above tests, specimens are not deformed plastically to a level normally achieved
in rolling operation. Therefore, some additional tests have been developed to evaluate
lubricity of oil under deforming workpiece condition. The two commonly known tests
under this category are Forming Test and Ring Compression Test. Some of these lubricity
tests are discussed below.
(a) Plint Tribometer Test: A reciprocating tribometer is used primarily for evaluation of
lubrication characteristics of the oil. It is a computerised friction and wear test apparatus.
A test panel (hot band) is dipped in the oil and a standard pin slides (line contact) over the
panel under a given load and at a predefined frequency. The variables under the
experiments could be speed, load, stroke, and oil temperature. Lubricity is assessed
automatically by the computer in terms of friction coefficient and can be plotted against
Friction coefficient
0.20
0.15 Oil-B
0.10
0.05 Oil-A
0.00
100 150 200 250
Temperature, oC
Results achieved at Plint Tribometer are truly representative of the industrial performance
and can be used to study thermal stability of the oil. It is also used to study the wear
debris and chemical interactions between oil and metal surface.
Flat Rolling Lubrication
(b) Forming Test: The forming test consists of deforming a perforated steel washer held
on the load cell mounted test table of Falex Tapping Torque machine. The average
forming torque of the lubricant is an index of its performance. The test specimen is a 1.13
mm thick steel washer of precisely controlled dimensions and metallurgy. The forming
tool is ball-ended and is made of die steel. For each test lubricant, a new forming tool is
used.
The test procedure used for evaluating a lubricant consists in determining the average
forming torque of a test fluid and that of a reference fluid using same forming tool. The
forming efficiency is then calculated as given below.
Forming Efficiency (%) = (A / B) x 100
Where, A is average forming torque of the reference lubricant, and B is average forming
torque for the test lubricant.
(c) Ring Compression Test: It is basically a plain strain compression test to measure the
friction between platens and ring surfaces during compression with different lubricants.
The ring used for this purpose is made of mild steel, which is ground and polished. The
ratio of outer diameter, inner diameter and thickness of the ring is maintained at 6:3:2.
The candidate oil is applied over the ring in neat form at a temperature of about 50-60 oC.
Reduction is imparted to the ring in steps from 10% to 60% by pressing it on a universal
testing machine. In each step, the change in the internal diameter is plotted against the %
reduction in height or thickness of the ring. The curves so obtained are compared with the
standard coefficient of friction curves to obtain the average friction coefficient between
the platen and the ring specimen.
(d) Evaluation of Oil Film Strength: The measurement of oil film strength is done
through an Optical
Incident light Detection
Rig Interferometer. 1 2
The schematic
diagram of the
method is shown in Glass disk
method, an oil film is generated between a steel ball and a glass disc having semi-
reflective coating. Film thickness is measured under different loads and speeds by
detecting the refracted/reflected light.
It has been observed that the 4 Ball EP Tester also gives a fairly good result with respect
to load bearing capacity of the oil. The critical load at which scar generates on three
stationary balls along with scar diameter gives the maximum load bearing capacity of the
oil. Weld load is also evaluated to measure the EP property of the oil.
Flat Rolling Lubrication
(e) Evaluation of Burn-off Characteristic: Cold rolling oils are designed for clean
burn-off during annealing process. The carried over oil from the mill should get
evaporated from the coil at lower temperature, say at about 400 oC without leaving any
100
75
Weight of Oil, %
50
25
0
0 200 300 400 500
Temperature, oC
residue. At the same time it should have sufficient thermal stability to sustain the roll bite
conditions. This property of the oil is studied through thermogravimetric analysis (TGA).
In this a known quantity of the oil is heated under controlled atmosphere and weight loss
is noted at increasing temperature (Figure 5.3). Since this test is conducted at atmospheric
pressure, it does not evaluate thermal stability of the oil at roll bite conditions. Even if
onset point for the distillation curve is between 200-250 oC, this does not mean that the
oil will decompose at roll bite. During the rolling process, the oil composition may be
unaffected by component loss due to the roll bite pressure being sufficiently higher than
the vapour pressure of even the most volatile components. In addition, chemical integrity
is maintained by selection of thermally and biologically hard raw material in conjunction
with a selected blend of antioxidants.
TGA can also be used to study the compatibility of general mill lubricants (morgoil,
hydraulic oil etc.) with the rolling oil. If a lubricant shows inferior burn-off characteristics
than the rolling oil, it may contaminate the annealed strip surface.
Chapter V Lubricant Management
(f) Evaluation of Rust Prevention Property: Rust prevention property of rolling oil is
studied in a humidity cabinet test. The samples of steel panels coated with 5% emulsion
are kept in humidity cabinet, with 100% humidity at 49 oC, for 48 hours. The samples are
examined before and after the test for any rust formation.
(g) Evaluation of Corrosiveness of Oil: The fatty acids present in rolling oil may cause
corrosion on mill equipment. The corrosiveness of the oil is evaluated in chemical attack
test, where test specimens of 1"x2" AISI 52100 chrome ball bearing steel are kept in neat
oil at 150oC for 24 hours. The surface of the balls is examined optically before and after
the test. The oil is rated according to the severity of the attack.
(h) Evaluation of Stability of Neat oil: Rolling oil is kept for seven days at 0 oC and is
examined for any defects in the oil upon cooling to room temperature. Again oil is kept
for 3 days at 80oC and is examined for any instability at 80oC or when it returns to room
temperature.
(i) Plate-Out Characteristics: It indicates the ability of the oil to come out of the
emulsion and properly spread in the roll bite. To evaluate this, steel samples are cleaned
and polished and dipped in emulsion of 3 and 5% oil concentration at 50 oC and then
dried and submerges in 1% copper sulphate solution for 5 seconds. Any copper adhering
to steel would indicate failure of the oil to spread evenly over the steel surface.
methodology which has been used to evaluate industrial applicability of various rolling
oils. The results obtained at the laboratory mill have been validated at industrial mill.
This methodology has been useful in developing large number of successful cold rolling
oils. Details of the laboratory rolling mill, the authors have extensively used for
development of these oils, are given in Annexure III.
At this mill, emulsion is prepared in a tank with varying oil concentration (1-5 % v/v) and
Temperature, oC
Cooling efficiency 100
of the oil is 80
measured in terms
60 Oil-A Oil-B
of emulsion and
40
sheet temperature
30 40 50 60 70 80 90
after rolling.
Cumulative Reduction, %
Cooling efficiencies
of two oils have Figure 5.5 Cooling characteristic of oil at
laboratory mill
been compared in
figure 5.5.
(d) Cleanliness Behaviour: Cleanliness of the mill and strip can be visibly observed
during rolling in the experimental mill. Surface reflectance of the rolled sheets, measured
in a tape test with the help of a reflectometer, is however a better way of quantifying
surface cleanliness of rolling oil. In this method first of all an adhesive scotch tape is
pasted over a white paper. Its reflectance is measured with the reflectometer and set at
100. This is considered as reference for the quantification of cleanliness of rolled sheets.
Subsequently, the tape is pasted over the rolled sheets and after removing from the sheet
it is again pasted over the white paper. During removal of the tape from the rolled sheet it
Flat Rolling Lubrication
carries with it all the loose deposits over the sheet. Reflectance of this tape is measured
and compared with that of the above reference.
The amount of carboneous deposit over rolled sheets before and after annealing can also
be measured using a surface carbon analyser. For this, a sample of the stained rolled sheet
is cut and placed in the sample boat inside the furnace of analyser. Temperature of the
furnace is set at 600 oC. Oxygen gas at controlled flow rate is then passed through the
furnace, which converts the surface carbon into carbon dioxide. Infrared cells present in
the analyser measures the quantity of carbon dioxide. From this the amount of carbon is
calculated and the result is displayed as milligram of carbon per unit area of the sample.
(e) Ageing Behaviour: The chemical ageing of rolling oil emulsion in the steel plant is
mainly due to tramp oil mixing, iron fine generation, impurity level in industry water and
bacterial growth. The same is generated in the experimental mill by mixing these
impurities in the emulsion tank. This impure form of emulsion is heated, agitated and
circulated for few weeks in the mill and then again a similar set of rolling is conducted as
is conducted with fresh emulsion. The difference in rolling parameters and emulsion
behaviour gives the idea of how particular oil deteriorates after a certain chemical ageing.
(b) Cooling Efficiency: The cooling potential of the oil is evaluated in terms of strip
temperature and work roll temperature. Roll thermal profile is also studied by measuring
work roll temperature along its barrel length.
(c) Surface Cleanliness: Reflectance of the cold rolled strips, iron fine deposit on the
strip, carbon and ash residues and thermal stability of the neat oil are selected as
parameters for evaluating the cleanliness properties of the candidate oil. The method of
measuring strip surface reflectance is the same as explained in case of laboratory
evaluation. It is generally studied at three locations, i.e. after rolling, after annealing, and
after skin pass rolling.
(e) Techno-economic Performance: The ultimate suitability of the candidate oil depends
on the techno-economics of its use and therefore it is evaluated in terms of rolling rate,
specific oil consumption, specific roll consumption, roll spalling, occurrence of strip
breakage, power consumption, etc.
provide a constant flow, temperature, pressure, particle size, pH and hardness of the
rolling solution.
The lubricant application systems have direct effect on cold rolling lubrication. For a
given mill and rolling oil, optimum design parameters may lead to improvement in its
effectiveness. The coolant flow rate and its distribution along the roll barrel length should
be properly calculated considering the requirements of both cooling and lubrication. The
total quantity of emulsion flow regulates the lubricity and the thermal condition at roll
bite. It varies from mill to mill and from stand to stand in a tandem mill depending upon
the softness of metal. The flow rate should be designed in such a way that the strip
temperature in no case exceeds 150 oC and there is no occurrence of frictional pick up.
The impact pressure of spray over the rolls affects the heat transfer coefficient; it
increases with increasing pressure to an optimum level after that it becomes constant. At
very high pressure, the spray bounces over the roll making it ineffective. The pattern of
flow along the work roll axis is also important because it may required to be varied
depending upon the differential deformation along the width of strip. The headers are
usually divided in different zones to facilitate control over emulsion flow. It helps in
controlling the shape of the rolled strip.
The rheology and film formation at roll bite very much depend on the temperature and
initial concentration of emulsion. Temperature control is important as its fluctuations
change the lubrication properties of the oil and lead to inconsistency in the rolling
process. The application system is designed with the possibility of changing the volume
fraction of oil.
The emulsions are mechanically sheared by agitator, pump and nozzles to achieve the
required particle size. The level of agitation depends on the type of emulsion oil. A stable
type emulsion requires less agitation to favour the self-cleaning action. However, higher
agitation is required for dispersion type oil to control its uniformity and the system must
be designed to avoid idle or dead spots within the system.
Chapter V Lubricant Management
In the injection method, rolling oil is injected into the existing roll cooling water sprays.
This method can be suitable for a new mill, which is designed with this feature. In an
existing mill, this method may not be practical as it increases the complexity of pipe-
work. Since all the rolling oil mixed with large volume of cooling water may not be
effectively utilised for lubrication purpose, this method has a big disadvantage of higher
oil consumption requirement.
Flat Rolling Lubrication
L
G
C F H
E L
B D
M
In a hot strip mill, roll wear is more pronounced at the early stands of finishing train. This
is why roll lubrication is provided at these stands (usually first three or four stands of a
six-stand finishing mill). This also ensures that any excess oil left over the rolled strip is
completely burnt off before the strip is cooled and coiled.
As shown in figure 5.6, mixing of oil and water is achieved in a simple device consisting
of a pipe elbow in the water line with the oil pipe attached so as to feed the oil axially
into the exit limb of the elbow. Water is flowing continuously and the oil is injected only
when a strip is being rolled. A non-return valve is provided in the oil line to keep it
primed. Generally alternate spray headers are provided for narrow and wider coils so that
unnecessary oiling of unused barrel length is avoided during rolling of narrow coils.
Desired values of some of these parameters are given in Table 5.4. These parameters are
measured either with the available equipment or by chemical methods.
(c) Emulsion pH: Emulsifier system of the rolling oil is normally pH sensitive. It is
therefore desirable that pH of the emulsion be controlled within a narrow specified range.
Acid carryover from the pickling line, inferior quality of feed water and mixing of tramp
oil are prime sources of pH deviation in the emulsion. In case, pH of the emulsion is not
controlled properly, it will lead to destabilised emulsification characteristics of the oil.
The preferred pH could range between 5.0 and 7.0; at pH values below this range, the
particle size distribution will increase as demonstrated by increased instability. Corrosion
problems and erratic rolling performance can be symptomatic of this condition. At pH
values above 7.0, the formation of metallic soaps is encouraged and also a reduction in
particle size is possible.
Chapter V Lubricant Management
the ions of low mass or high charge, e.g. H +, OH-, Cl-, and SO42-. Minor contributors
The conductivity is dependent on the make up water. Good quality deionised water will
have a conductivity of less than 10 mho, while poor quality industrial water can have
conductivity even above 500 mho. An increasing concentration of salt from the hard
water decreases the emulsion stability. Another source of salt (e.g. chloride) is carryover
from pickling line. The chloride level in the final rinse of pickling line should be
controlled within 60 ppm. Carryover of chloride should not be allowed to exceed 0.03
mg/sq.ft of pickled strip. Conductivity of rolling oil emulsion is normally checked within
200 S/cm and in no case it should exceed 500 S/cm.
Flat Rolling Lubrication
(e) Oil particle size: The most important emulsion parameter that controls both lubricity
and emulsification characteristics is oil particle size. A typical distribution of oil particle
size in an emulsion is shown in figure 5.7 and its typical range observed with some
successful cold rolling oils is given in Table 5.5. The oil particle size depends upon many
factors. The type and dose of emulsifier is the major controlling element of oil particle
size. Apart from this, there are several other external factors that affect the particle size.
Important among them are - type of filtration, size of system, retention time, emulsion
temperature, type of water used, system configuration, spray pressure, types of
contaminants, and type of material being rolled. For its control, however, adequate
agitation should be applied on the emulsion depending upon the type of rolling oil
(unstable, metastable, stable). In absence of particle size analyser, emulsion stability
index (ESI) should be measured periodically.
10
8
Volume, %
6
4
2
0
0 2 4 6 8 10 12 14 16 18
Droplet size, micron
Figure 5.7 Oil Droplet size in emulsions of rolling oils
(f) Tramp Oil: The tramp oil must be removed from the rolling oil solution periodically
to improve its health. The modern oils are having tramp rejecting characteristics and
therefore it is easy to remove the tramp oils by skimming it off. In no case it should be
allowed to increase over 20-30% level. It is calculated by measuring sap value of
extracted oil.
Table 5.5 Typical oil particle size and other related parameters
Chapter V Lubricant Management
(g) Iron in Emulsion: Iron content in the solution should be maintained less than 200
PPM with the use of magnetic separator. Other foreign bodies should also be removed
from the solution with the use of filtration system to avoid any strip surface
contamination.
(h) Bacterial Count: The bacterial attack on the emulsion can lead to build-up of acidic
materials, enhanced corrosiveness (a fall in pH), destruction of additives, foul odour, loss
of stability in emulsions (increase in oil particle size), increase in free oil and oil
consumption, and/or excessive foaming. The alarming levels of bacteria and yeasts
(i) Analysis of Extracted Oil: The emulsion quality of a rolling oil in use at an industrial
mill can be assessed at different interval of time by extracting the oil phase from the
emulsion and determining some of its properties. These properties include free fatty acid,
acid number, and saponification value. Oil extraction is done not chemically but with the
help of mechanical equipment such as rotary evaporator so that dry and unreacted oil is
obtained for further analysis.
The acid value of the extracted oil will usually be lower than that of the fresh oil. Free
fatty acids (FFA) are lost due to soap formation with iron and water hardness salts. Any
mineral oil contamination of the emulsion will also reduce the % of FFA present. If the
acid value increases suddenly this could be caused by excessive bacterial activity
resulting in the formation of short chain degradation products o hydrolysis of ester due to
live steam leak, etc.
Flat Rolling Lubrication
The drop in Sap value usually indicates contamination of emulsion with the tramp oils. It
is used to calculate the presence of active oil in the emulsion.
Active Oil (%) = [(Sap of extracted oil) / (Sap of fresh oil)] x 100
Although the % active oil varies from mill to mill, as a general rule, it is not allowed to
fall below 70%. The level of tramp oil is calculated from active oil as,
Tramp oil = Total oil – Active oil
Infrared analysis of the extracted oil is also done to predict its ester content and fatty acid
concentration. It also finds its application in identification of contamination in emulsion
and monitoring changes in oil composition during storage as well as in use.
5.5
Troubleshooting in Cold Rolling Mills
The cold rolling process is complex and it is often difficult to establish the cause of
problem. It is suggested that regular monitoring of process and emulsion parameters
should be conducted to establish a set of reference results. Upper and lower control limits
should also be set for these parameters to trigger corrective actions and thus limit the
number of problems. Some of the condition-monitoring methods are suggested in Table
5.6 for different troubleshooting purposes.