Nano Additives Based Lubricants

Product name:
LUBRICANT WITH LAYERED NANOSTRUCTURE ADDITIVES
Abstract:
The present subject matter provides a method (100) for preparing a lubricant with layered
nanostructure additives. The method (100) comprises the steps of contacting the layered
nanostructure additives with a surfactant and a solvent to obtain a first mixture, evaporating
the solvent from the first mixture to obtain surface modified layered nanostructure additives,
and dispersing the surface modified layered nanostructure additives in a lubricating fluid to
obtain the lubricant. The lubricating fluid comprises base oil in a range of 90-99% by weight
of the lubricating fluid and additives in a range of 1-10% by weight of the lubricating fluid.
The layered nanostructure additives dispersed are selected from the group consisting of
nanoplatelets, nanoflowers, and a combination thereof and the weight ratio of the surfactant
to the layered nanostructure additives is in a range of 1.2:1 to 1.5:1.
FORM 2
THE PATENTS ACT, 1970 (39 of 1970) & THE PATENTS RULES, 2003
COMPLETE SPECIFICATION (See section 10, rule 13) 1. Title of the invention:
LUBRICANT WITH LAYERED NANOSTRUCTURE ADDITIVES
2. Applicant(s)
NAMENATIONALITY ADDRESS
HINDUSTAN PETROLEUM Indian Petroleum House, 17, Jamshedji

CORPORATION LIMITED Tata Road, Churchgate, Mumbai
Maharashtra, 400020, India
3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it
is to be performed.
TECHNICAL FIELD
[0001] The present subject matter relates, in general, to additives for lubricants
and, in particular, to layered nanostructure additives for lubricants.
BACKGROUND
[0002] Friction and wear between moving mechanical components of machines and
automobiles often result in energy and material losses. Lubricants are substances which are
introduced between surfaces in mutual contact to reduce friction between them. In
automobiles, lubricants keep surfaces of moving components separated, thus reducing friction
and wear, and thereby increasing mechanical durability, energy efficiency of various
components of the automobile, and longevity of the components. Lubricants also act as
coolants to remove heat produced by friction. They also coat surfaces of moving mechanical
components and protect them from wear and corrosion. In order to provide these functions,
lubricants typically comprise one or more additives or property modifiers in addition to base
oil. These additives can be, for example, antioxidants, detergents, anti-wear substances, anti-
foaming agents, viscosity index improvers, and the like.

BRIEF DESCRIPTION OF DRAWINGS
[0003] The detailed description is described with reference to the
accompanying figures. In the figures, the left-most digit(s) of a reference number identifies
the figure in which the reference number first appears. The same numbers are used
throughout the drawings to reference like features and components. For simplicity and clarity
of illustration, elements in the figures are not necessarily to scale.
[0004] Fig. 1 illustrates
a method for preparing layered nanostructure additive based lubricants, in accordance
with an implementation of the present subject matter.

[0005] Fig. 2 graphically
illustrates HR-SEM images of the layered nanostructure additives, in accordance

[0006] Fig. 3(a) illustrates wear test results for the layered nanostructure additive based
lubricant with diesel engine oil as the lubricating fluid at a load of 40 kgf, in accordance with
an implementation of the present subject matter.
[0007] Fig. 3(b) illustrates wear test results for the layered nanostructure additive based
lubricant with diesel engine oil as the lubricating fluid at a load of 60 kgf, in accordance with
[0008] Fig. 3(c) illustrates wear test results for the layered nanostructure additive based
lubricant with petrol engine oil as the lubricating fluid at a load of 40 kgf, in accordance with
[0009] Fig. 3(d) illustrates wear test results for the layered nanostructure additive based
lubricant with petrol engine oil as the lubricating fluid at a load of 60 kgf, in accordance with

[0010] Fig. 3(e) illustrates wear test results for the layered nanostructure additive based
lubricant with gear oil of GL 4 grade and viscosity SAE 80W90 as the lubricating fluid at a
load of 40 kgf, in accordance with an implementation of the present subject matter.
[0011] Fig. 3(f) illustrates wear test results for the layered nanostructure
additive based lubricant with gear oil of GL 4 grade and viscosity SAE 80W90 as the
lubricating fluid at a load of 80 kgf, in accordance with an implementation of the present
subject matter.
[0012] Fig. 3(g) illustrates wear test results for the layered nanostructure additive based
lubricant with gear oil of GL 4 grade and viscosity EP140 as the lubricating fluid at a load of
40 kgf, in accordance with an implementation of the present subject matter.
[0013] Fig. 3(h) illustrates wear test results for the layered nanostructure additive based
lubricant with gear oil of GL 4 grade and viscosity EP140 as the lubricating fluid at a load of
80 kgf, in accordance with an implementation of the present subject matter.

[0014] Fig. 4(a) graphically illustrates friction test results indicating the variation in
coefficient of friction of the layered nanostructure additive based lubricant with diesel engine
oil as the lubricating fluid, in accordance with an implementation of the present subject
matter.
[0015] Fig. 4(b) graphically illustrates seizure load results indicating the variation in seizure
load of the layered nanostructure additive based lubricant with diesel engine oil as the
lubricating fluid, in accordance with an implementation of the present subject matter.

[0016] Fig. 4(c) graphically illustrates friction test results indicating the variation in
coefficient of friction of the layered nanostructure additive based lubricant with petrol engine
oil as the lubricating fluid, in accordance with an implementation of the present subject
matter.
[0017] Fig. 4(d) graphically illustrates seizure load results indicating the variation in seizure
load of the layered nanostructure additive based lubricant with petrol engine oil as the
lubricating fluid, in accordance with an implementation of the present subject matter.

[0018] Fig. 4(e) graphically illustrates friction test results indicating the variation in
coefficient of friction of the layered nanostructure additive based lubricant with gear oil of
GL 4 grade and viscosity SAE 80W90 as the lubricating fluid, in accordance with an
implementation of the present subject matter.
[0019] Fig. 4(f) graphically illustrates seizure load results indicating the variation in seizure
load of the layered nanostructure additive based lubricant with gear oil of GL 4 grade and
viscosity SAE 80W90 as the lubricating fluid, in accordance with an implementation of the
present subject matter.

[0020] Fig. 4(g) graphically illustrates friction test results indicating the variation in
coefficient of friction of the layered nanostructure additive based lubricant gear oil of GL 4
grade and viscosity EP140 as the lubricating fluid, in accordance with an implementation of
the present subject matter.
[0021] Fig. 4(h) graphically illustrates seizure load results indicating the variation in seizure
load of the layered nanostructure additive based lubricant with gear oil of GL 4 grade and
viscosity EP140 as the lubricating fluid, in accordance with an implementation of the present
subject matter.
[0022] Fig. 5(a) graphically illustrates extreme pressure (EP) test results indicating the
variation in Load wear index (LWI) of the layered nanostructure additive based lubricant
with gear oil of GL 4 grade and viscosity SAE 80W90 as the lubricating fluid, in accordance

[0023] Fig. 5(b) graphically illustrates the extreme pressure (EP) test results
indicating the variation in weld load of the layered nanostructure additive based lubricant
with gear oil of GL 4 grade and viscosity SAE 80W90 as the lubricating fluid, in accordance

[0024] Fig. 5(c) graphically illustrates the extreme pressure (EP) test results
indicating the variation in Load wear index (LWI) of the layered nanostructure additive based
lubricant with gear oil of GL 4 grade and viscosity EP140 as the lubricating fluid, in
accordance with an implementation of the present subject matter.
[0025] Fig. 5(d) graphically illustrates the extreme pressure (EP) test results
indicating the variation in weld load of the layered nanostructure additive based lubricant
with gear oil of GL 4 grade and viscosity EP140 as the lubricating fluid, in accordance with
[0026] Fig. 6 graphically illustrates characterization of worn out balls using a
scanning electron microscope with X-ray diffraction attachment for the layered nanostructure
additive based lubricant, in accordance with an implementation of the present subject matter.
[0027] Fig. 7 graphically illustrates variations in brake thermal efficiency of the layered
nanostructure additive based lubricant in a diesel engine test rig, in accordance with an
implementation of the present subject matter.

[0028] Fig. 8 graphically illustrates variation in total fuel consumption of the layered
nanostructure additive based lubricant, in accordance with an implementation of the present
subject matter.
DETAILED DESCRIPTION
[0029] Generally, on fractional distillation of crude oil, different base oils separate out as
distillates. Examples of base oils are petroleum distillates, mineral oils, vegetable oils, esters,
polyolefin, etc. Typically, formulations of lubricants comprise base oil and additives.
[0030] Nanoparticles have been tested for use as additives in the base oils for lubricants in
automobile and other industrial applications. These nanoparticles may be metallic, non-
metallic, or salts of metals and non-metals having an average particle diameter upto 100 nm.
Studies have shown that nanoparticle based lubricants exhibit better tribological properties as
compared to ordinary lubricants without nanoparticles due to their nano size. Their small size
also enables them to penetrate into wear crevices. Nanoparticles have a high surface to
volume ratio which imparts high surface affinity and chemical reactivity to the nanoparticles.
They can also form a thin coating with the thickness of just one or two molecules to separate
surface asperities of the moving components of a machine. Thus, nano particles are emerging
as suitable additives for industrial lubricants, such as, lubricating engine oils, greases, dry
film lubricants, and forging lubricants.
[0031] Several types of nanoparticles have been studied as potential additives for
lubricants, including metal oxides of silicon, titanium, nickel, tin, aluminium, and zinc;
fluorides of metals such as cerium, lanthanum, and calcium; and zinc, tin, and lead sulfides,
and metals, such as nickel, zinc, tin, and silver, and non-metals like carbon nanotubes.
Nanoparticles may also be of different types based on their structure, for example,
nanospheres, nanoplatelets, and nanoflowers. Nanoplatelets have a layered nanostructure
which comprise of stacks of nanomaterial, predominantly nanosheets. The stacks vary in
thickness from 1-15 nm and have an average diameter of 1-100 micrometer. Nanoflowers
also comprise a layered nanostructure and have a flower-like morphology when visualized
under a microscope.
[0032] As both nanoplatelets and nanoflowers comprise stacks that are bound to
each other by weak Vander Waal’s force, these stacks tend to slide over each other. This
provides ready partial cleavage of the stacks under rubbing conditions, providing high
resistance to friction and wear and extended lifetime in vacuum.
[0033] Lubricating properties of fully formulated lubricating fluids may be enhanced by
dispersing these layered nanostructure additives, such as nanoplatelets and nanoflowers, in
lubricating fluid, for example, petrol engine oil of SM grade, diesel engine oil of CI 4 grade,
and gear oil GL 4 grade. These lubricating fluids include base oils and other additives, such
as, detergents, anti-foaming agents, antioxidants, and the like, that have different property
modifying effects which make them suitable for use as lubricants.
[0034] However, these layered nanostructure additives in fully formulated lubricants tend to
agglomerate due to the presence of other additives, such as antioxidants, detergents, and the
like, which are already present in the lubricant. Agglomeration caused by the other additives
tends to destabilize the dispersion making the lubricant unsuitable and causing potential
damage to moving components. Moreover, the other additives in the lubricating fluid tend to
cause shearing of the stacks in the layered nanostructure further
leading to destabilization of the nanostructures in the lubricating fluid. Therefore, the
challenge is to obtain a layered nanostructure additive based lubricant which has a uniform
dispersion of the layered nanostructure additives in the fully formulated lubricating fluid and
which does not agglomerate or settle over an extended period of time.
[0035] The present subject matter provides a method for preparing a lubricant
with layered nanostructure additives. The method comprises the steps of contacting the
layered nanostructure additives with a surfactant and a solvent to obtain a first mixture,
evaporating the solvent from the first mixture to obtain surface modified layered
nanostructure additives, and dispersing the surface modified layered nanostructure additives
in a lubricating fluid to obtain the lubricant. The lubricating fluid comprises base oil in a
range of 90-99% by weight of the lubricating fluid and other additives in a range of 1-10% by
weight of the lubricating fluid. The layered nanostructure additives dispersed in the
lubricating fluid are selected from the group consisting of nanoplatelets, nanoflowers, and a
combination thereof and the weight ratio of the surfactant to the layered nanostructure
additives is in a range of 1.2:1 to 1.5:1.
[0036] The method provides a stable suspension of layered nanostructure additives, namely
nanoplatelets and nanoflowers, in the lubricating fluid. The lubricant obtained by the method
also shows improved performance characteristics, such as anti-wear, anti-friction, and
extreme pressure characteristics when compared to lubricants without the layered
nanostructure additives as will be explained later with test results. Thus, layered
nanostructure additives can be dispersed in a stable manner in lubricating fluids comprising
base oil and additives, to form the layered nanostructure additive based lubricant.
[0037] These and other advantages of the present subject matter will be described in greater
detail in conjunction with the figures as illustrated. It should be noted that the description and
figures merely illustrate the principles of the present subject matter and in no way limit the
present subject matter to the description and figures illustrated herein.

[0038] Fig. 1 illustrates a method 100 for preparing a lubricant with 4 layered
nanostructure additives, in accordance with an implementation of the present subject matter.
The method 100 includes contacting the layered nanostructure additives with a surfactant and
a solvent to obtain a first mixture, at block 102. The layered nanostructure additives may
have different morphologies. For instance, the layered nanostructure additives may be
nanoplatelets and nanoflowers. The nanoplatelets and nanoflowers of the present subject
matter have a thickness varying between 5-10 nm. It has been tested that the nanoplatelets
and nanoflowers with thickness over the mentioned range exhibit optimal lubricating
properties, as will be explained later. Layered nanostructure additives having greater
thickness may be subject to shearing which adversely affects the stability of the lubricant. In
an example implementation, the layered nanostructure additives used for the method 100 may
be selected from one of transition metal disulphides, graphene, inorganic graphene analogues,
and combinations thereof. In an example implementation, the transition metal disulphides are
selected from the group consisting of molybdenum disulphide, tungsten disulphide, and
combination thereof.
[0039] At block 102, the layered nanostructure additives are contacted with the
surfactant and the solvent to obtain a first mixture. In one implementation, the solvent is
selected from the group consisting of hexane, iso-octane, n-heptane, toluene, and the like. For
stability in a fluid medium, the surface of the layered nanostructure additives needs to be
suitably modified with the surfactant. The surfactants include compounds that lower the
surface tension between two liquids or a liquid and a solid and may be used as detergents,
anti-foaming agents, and dispersants. When the surfactants are mixed with the layered
nanostructure additives, one end of the surfactant molecule attaches to the surface of the
layered nanostructure additives through chemical bonds. The other end of the surfactant
molecule is free and extends into the lubricating fluid forming reverse micelles. Thus, the
surfactants generate an effective repulsive force between layered nanostructure additives due
to steric repulsion between the surfactant molecules attached to the surface of
the nanostructures, thereby
preventing agglomeration. The effective repulsive force between the layered nanostructure
additives coated with the surfactant results in a stable mixture of the layered nanostructure
additives in the lubricating fluid. In one implementation, the surfactant is selected from the
group consisting of sorbitan monooleate (SPAN 80), cetyl trimethylammonium bromide
(CTAB), and a combination thereof. In an implementation, the weight ratio of the surfactant
to the layered nanostructure additives is in a range of 1.2:1-1.5:1. It has been tested that this
weight ratio of the surfactant to the layered nanostructure additives did not increase the
foaming tendency of the lubricant, as will be explained later. In one implementation, a
mixture of the layered nanostructure additives and the surfactant is dissolved in the solvent to
form the first mixture.
[0040] The method 100, at step 104 includes, evaporating the solvent from the first mixture
to obtain the surface modified layered nanostructure additives. Evaporating the solvent from
the first mixture improves enhancement of reverse micelle formation by improving surface
bonding of the surfactants to the layered nanostructure additives. In an example
implementation, the method comprises sonicating the first mixture prior to evaporating the
solvent. The first mixture can be sonicated in an ultrasonic probe sonicator at 50 % amplitude
in pulse mode for 30 minutes followed by sonication in continuous mode for 30 minutes for
thorough mixing, formation, and bonding of reverse micelles to the surface of the layered
nanostructure additives. The sonication of the first mixture prior to evaporating the first
mixture causes the reverse micelles to properly bond to the surface of the layered
nanostructure additives, thereby increasing stability of layered nanostructure additives in the
lubricating fluid.
[0041] Evaporating the solvent, at block 102, includes stir heating on a magnetic stirrer. In
an implementation, the stir heating is conducted on the magnetic stirrer at a speed of 500-600
rpm and at a temperature range of 60-70oC. The stir heating helps in removing any excess
solvent molecules trapped in the nanostructure of the layered nanostructure additives and also
superficially modifies the surface of the layered nanostructure additives
by one of chemisorption and functionalization, thereby increasing lipophilicity of the
layered nanostructure additives. This further increases stability of the layered nanostructure
additives when dispersed in the lubricating fluid. The surface modified layered nanostructure
additives obtained from evaporating the solvent, at block 102, may be cooled and dried to
obtain a fine powder of the surface modified layered nanostructure additives which may be
packed and stored or dispersed in the fully formulated lubricating fluid.
[0042] The method 100, at step 106, includes dispersing the surface modified
layered nanostructure additives in the lubricating fluid to obtain the lubricant. The lubricating
fluid comprises base oil in a range of 90-99% by weight of the lubricating fluid and other
additives in a range of 1-10% by weight of the lubricating fluid. The additives present in the
lubricating fluid may include corrosion inhibitors often used in engine coolant like boron,
alkaline or detergent additives, such as magnesium and calcium used to neutralize acids
which form during a combustion process in an engine, a friction-reducer and anti-oxidant,
such as molybdenum, an anti-foaming agent, such as silicon, and an anti-oxidant and anti-
wear agent, such as Zinc dialkyl dithio phosphate (ZDDP). The lubricating fluid contains the
above mentioned elements as additives for functioning under severe conditions.

[0043] At step 106, dispersing the surface modified layered nanostructure additives
in the lubricating fluid includes contacting the surface modified layered nanostructure
additives with the lubricating fluid to form a first suspension and sonicating the first
suspension to obtain the lubricant. In an example implementation, sonicating the first
suspension includes ultra sonicating, in an ultrasonic probe sonicator, for a time period of 8-
12 minutes at 50% amplitude under a pulse mode of 0.5 seconds. This is followed by
sonication in continuous mode for 30 – 40 minutes. For optimal stability of the layered
nanostructure additives in the lubricant, sonicating the first suspension comprises ultra
sonicating, in an ultrasonic probe sonicator, for a time period of 10 minutes at 50%
amplitude under a pulse mode of 0.5 seconds followed by sonication in
continuous mode for 30 minutes. Sonicating improves dispersion of the layered nanostructure
additives in the lubricant and increases stability of layered nanostructure additive based
lubricant.
[0044] The present subject matter also provides a lubricant dispersed with surface
modified layered nanostructure additives. The lubricant comprises the lubricating fluid
comprising about 90% to 99% base oil and about 1% to 10% additives and surface modified
layered nanostructure additives from about 0.05 weight % to 0.2 weight % dispersed in the
lubricating fluid. The layered nanostructure additives are selected from the group consisting
of nanoplatelets, nanoflowers, and a combination thereof. The layered nanostructure additives
are fabricated from a material selected from the group consisting of transition metal
disulphides, graphene, inorganic graphene analogues, and combinations thereof.
[0045] The following discussion is directed to various examples of the present subject
matter. Although certain methods and compositions have been described herein as examples,
the scope of coverage of this patent application is not limited thereto. On the contrary, the
present subject matter covers all methods and compositions fairly falling within the scope of
the claims either literally or under the doctrine of equivalents.
[0046] Certain terms are used throughout the description to refer to certain components and
are to be construed as being mentioned by way of example and for purposes of explanation
and not as limiting.
[0047] The term “viscosity index” as used in the examples refers to change in
viscosity of a lubricant with change in temperature. The lower the viscosity index, the greater
is the change of viscosity of a lubricant with temperature. Thus, the higher the viscosity
index, the better is the quality of the lubricant. A viscosity index value greater than 90 is
preferred for the lubricant.
[0048] The term “American Society for Testing and Materials (ASTM) D 445” as used in the
examples refers to a test method that specifies a procedure for determination of kinematic
viscosity of the lubricant by measuring the time for a volume of liquid to flow under gravity
through a calibrated glass capillary viscometer.
[0049] The term “total acid number” (TAN) ASTM D 664 as used in the examples
determines ability of lubricant to resist additive depletion, acidic contamination and oxidation
of lubricant under automotive environment. The TAN is the amount of potassium hydroxide
in milligrams required to neutralize the acids in one gram of the lubricant. The TAN value
indicates potential corrosiveness of the lubricant. A TAN value lesser than 3 indicates that the
lubricant is stable.
[0050] The term “total base number” (TBN) as used in the examples refers to effectiveness of
the lubricant in controlling acid formation during combustion process. The higher the TBN,
the more effective the lubricant is in suspending wear-causing contaminants and reducing the
corrosive effects of acids over an extended period of time. A TBN value higher than 5
indicates that the lubricant has good control over acid formation during the combustion
process.
[0051] The term “ASTM D 2896” as used in the examples refers to a test method for
determination of the TBN of the lubricant by potentiometric titration with perchloric acid in
glacial acetic acid.
[0052] The term “ASTM copper strip corrosion standard as per ASTM D 130” as used in the
examples refers to a standard used for representing corrosion protection of the lubricant. The
standard has classification numbers from 1 to 4 for various color and tarnish levels of a
copper strip immersed in the lubricant. A classification number of 1a indicates excellent
corrosion protection, 1b indicates good corrosion protection, and 1c indicates sufficient
corrosion protection of the lubricant.
[0053] The term “copper strip corrosion test” as used in the examples refers to a
test used for determining the classification number of the lubricant. The test involves
immersion of a polished copper strip in the lubricant at elevated temperature for a
period of time and testing the color and tarnish levels of the copper strip.
[0054] The term “four-ball wear test machine” as used in the examples refers to a
machine used for testing various performance characteristics of the lubricant. The machine
comprises of a ball pot in which three balls are clamped together and thereby kept stationary
or fixed in one position. These balls are then covered with the lubricant. A fourth ball is
pressed against a cavity formed by the three stationary balls and the fourth ball is rotated.
[0055] The term “wear scar diameter” as used in the examples refers to diameter of wear
scars on the three stationary balls tested on the four-ball wear test machine. The larger the
wear scar, the poorer is the lubricating ability of the lubricant.

evaluation of the anti-wear properties of the lubricants in sliding contact by means of the
Four-Ball Wear Test Machine.
[0057] The term “seizure load” as used in the examples refers to a load at which a sudden
increase in coefficient of friction value occurs. The higher the seizure load, the better the anti-
friction property of the lubricant.
determining coefficient of friction of the lubricant by means of the Four-Ball Wear Test
Machine. Initially, a load is applied which gradually increased at regular time intervals until
the lubricant undergoes seizure.
[0059] The term “friction test” as used in the examples refers to a test performed for
determining the seizure load and the coefficient of friction of the lubricant. The seizure load
refers to the load at which there is a sharp rise in fractional torque characterized on a graph
while the machine is running. The coefficient of friction is determined by considering the
loads between initial load and the seizure load.
determination of the load-carrying properties of lubricating fluids. The following two
determinations are made using ASTM D 2783: 1. Load-wear index, and 2. Weld load by
means of the four-ball extreme-pressure tester.
[0061] The term “load-wear index” as used in the examples refers to an extreme pressure
(EP) property of the lubricant calculated using the four-ball wear test machine. Here the
speed of rotation is maintained at 1760 RPM and the whole test procedure is done under
room temperature. A series of tests of 10-s duration are carried out with increasing loads
during each tests until 4 balls weld under extreme pressure. The load at which weld occurs is
called the weld load. The first run is made at an initial load of 40 kgf and the additional runs
are carried out at consecutively higher loads until and the 4 balls weld under extreme
pressure. A total of 10 readings are considered in the test and the corrected load is calculated
for all ten readings. The load wear index is calculated from the corrected load. The corrected
load is calculated as follows:
Corrected load=LDh/X;
where L is the applied load in kgf, Dh is hertz scar diameter in mm, and
X is average scar diameter in mm.
Hertz scar diameter is the average diameter, in mm, of an indentation caused by deformation
of the balls under static load before application of the load. It may be calculated from the
equation Dh = 8.73X10-3 (P)1/3.
[0062] The term “endurance test” as used in the examples refers to a test conducted on an
engine by subjecting it to varying loads and varying speeds for a continuous period of 80
hours without stoppage. This is used to determine the engine wear & tear and fuel
consumption over a period of time.
[0063] The term “bench test” as used in the examples refers to a test
performed on the engine at a particular load and a particular speed to determine the efficiency
of the engine at that particular load and speed.
[0064]The term "petrol engine rig" as used in the examples refers to a test rig consisting of
petrol engine connected to a dynamometer for applying speed and loads to an engine.
[0065] The term "diesel engine rig" as used in the examples refers to test rig consisting of
diesel engine connected to dynamometer for applying speed and loads to an engine.
EXAMPLES
EXAMPLE 1: PREPARATION OF LUBRICANT WITH LAYERED NANOSTRUCTURE
ADDITIVES USING THE METHOD OF THE PRESENT SUBJECT MATTER
[0066] In an example implementation, the layered nanostructure additive
includes nanoplatelets of molybdenum disulphide, tungsten disulphide, and graphene. It is to
be understood that nanoplatelets and nanoflowers of other transition metals and graphene
analogues may be used. The nanoplatelets have a thickness ranging from 5-10 nm. At this
range, the nanoplatelets used in the lubricant provide optimal results. A High Resolution-
Scanning Electron Microscope (HR-SEM) analysis of the nanoplatelets was conducted. Fig. 2
depicts the HR-SEM images obtained by analysis of the nanoplatelets, in accordance with an
implementation of the present subject matter. In Fig. 2, 200a depicts HR-SEM image of
molybdenum disulphide nanoplatelets, 200b depicts the HR-SEM image of tungsten
disulphide nanoplatelets, and 200c depicts the HR-SEM image of the graphene nanoplatelets.
[0067] The surface of the nanoplatelets was modified using a surfactant to
prevent agglomeration of the nanoplatelets and to obtain a uniform dispersion of the
nanoplatelets in the lubricating fluid. In an example implementation, sorbitan monooleate is
selected as the surfactant for surface modification of the nanoplatelets. The nanoplatelets are
coated with the sorbitan monooleate surfactant to form the surface modified nanoplatelets. As
a result of the surface modification, reverse micelles of the surfactant are formed on the
surface of the nanoplatelets which increase stability of the lubricant by
preventing
agglomeration of the nanoplatelets. In the example implementation, the surface modified
nanoplatelets from about 0.05 weight % to 0.2 weight % were dispersed in the lubricating
fluid to obtain the lubricant. Dispersing the surface modified nanoplatelets at the mentioned
range provides optimal results of lubrication. Beyond the above mentioned range of weight %
of the surface modified layered nanostructure additives there may be an increase in wear
effects on mechanical moving components of an engine where the layered nanostructure
additive based lubricant is being used. This may be due to overcrowding of the surface
modified layered nanostructure additives at interfaces between the mechanical moving
components of the engine in relative motion.
[0068] In the example implementation, the sodium monooleate (SPAN 80) surfactant and the
nanoplatelets in ratio of 1.5:1 was mixed in approximately 50.0 ml of n-hexane solvent to
form a first mixture. The first mixture was sonicated in an ultrasonic probe sonicator for a
time period of 1 hour at 50% amplitude under a continuous mode followed by evaporation.
Evaporation was achieved by stir heating the sonicated first mixture on a magnetic stirrer at a
speed of 500-600 rpm and at a temperature range of 60-70oC to obtain the surface modified
nanoplatelets. The surface modified nanoplatelets were cooled and dried prior to dispersing in
a lubricant. The surface modified nanoplatelets were contacted with the lubricant to form a
first suspension and sonicated in an ultrasonic probe sonicator, for a time period of 10
minutes at 50% amplitude under a pulse mode of 0.5 seconds to obtain the lubricant. The
surface modified nanoplatelets were dispersed in lubricating fluids, such as GL-4 grade, SM
grade, and CI-4 grade lubricants. Compositions of the lubricating fluids are as illustrated in
Table 1. It is to be understood that any other lubricating fluid comprising base oil in a range
of 90-99% by weight of the lubricating fluid and additives in a range of 1-10% by weight of
the lubricating fluid may be used.
Table 1: Additive composition in HP GL-4, Racer 4, and HP CI 4 lubricants
Grade
HP GL -4 Racer 4 HP CI 4
a b c d e f g h Calcium, mg/Kg ASTM D5185 <10 1700 to 1900
3000 to 4000
Zinc , mg/Kg ASTM D5185 <10 800 to 1200 1000 to 1500
Phosphorous, mg/Kg ASTM D5185 100 to 200 700-1000 1000
to 1500
Sulfur, Wt% ASTM D4951 1 to 4 0.1 to 0.5 0.1 to 0.75
Magnesium , mg/Kg ASTM D5185 <10 <10 <10
Molybdenum, mg/Kg ASTM D5185 <10 <10 <10
Boron, mg/Kg ASTM D5185 <10 <10 <10
Sodium, mg/Kg ASTM D5185 5 – 20 10-16 10-20

[0069] In an example implementation, the layered nanostructure additive based lubricant
described herein can be used for lubrication in vehicles in the automotive industry. Thus, to
determine the suitability of the layered nanostructure additive based lubricant in the
automotive industry evaluation of physico-chemical properties of the layered nanostructure
additive based lubricant becomes necessary. The physico-chemical properties of lubricants
include viscosity index, total acid number, total base number, and the like, that determine the
suitability of lubricant for use in vehicles, such as in engines of two-wheelers and four-
wheelers. The physico-chemical properties of the layered nanostructure additive based
lubricants were evaluated to investigate the suitability of the surfactant and the surface
modification process to the automotive environment.
EXAMPLE 2: EVALUATION OF PHYSICO-CHEMICAL PROPERTIES OF THE
LUBRICANT COMPRISING SURFACE MODIFIED LAYERED NANOSTRUCTURE
ADDITIVES
[0070] In an example implementation to analyze the physico-chemical properties of
the layered nanostructure additive based lubricant, different tests such as foaming tendency
test, Kinematic viscosity test, total acid number test, total base number test, and copper strip
corrosion test were performed.
EXAMPLE 2.1: FOAMING TENDENCY TEST
[0071] Generally, lubricants comprise foaming additives. These foaming additives keep the
engine and other components clean by producing foam. However, excessive foam can result
in loss in lubrication which eventually leads to mechanical failure of the engine and its
components.
[0072] Surfactants used for surface modification of layered nanostructure additives often
generate foam and can increase the amount of foam produced by the lubricant. Therefore, the
foaming tendency of the layered nanostructure additive based lubricant was tested to assess
effect of the surface modified layered nanostructure additives on the foaming tendency of the
lubricant.
[0073] The foaming tendency was tested as per ASTM D 892 and was performed in two
stages. During the first stage, 200ml of a sample of the layered nanostructure additive based
lubricant was maintained at a temperature of 24oC in a 1000ml beaker. Air was constantly
blown through the sample at a constant rate of 95 mL/min for 5 minutes. The sample was
allowed to rest for 10 mins. Volume of foam was measures at the end of blowing of air and
after the sample was allowed to rest. During the second stage, a sample of the layered
nanostructure additive based lubricant was maintained at a temperature of 93.5oC. Air was
constantly blown through the sample at a constant rate of 95 mL/min for 5 minutes. The
sample was allowed to rest for 10 mins. Volume of foam was measured at the end of blowing
of air and after the sample was allowed to rest. The volume of foam generated for layered
nanostructure additive based lubricant for different ratios of surfactant to layered
nanostructure additives is as illustrated in Table 2.1.
Table 2.1: Results of foaming tendency test
Sample (Racer 4 as base oil-200mL) Ratio of
Surfactan
t to the
layered
nanostru
cture additives Foam Volume (ml)
First stage at 24 oC Second stage at 93.5 oC
At the end of
5 min
blowing
period At the end of 10 min settling period At the end of
5 min
blowing
period At the end of 10
min settling
period
Base oil 0 5 Nil 30 Nil
Base oil
+0.05 WS2
(CTAB) 1.5:1 5 Nil 30 Nil

Base oil + 0.05% WS2 (SPAN 80) 1.5:1 5 Nil 32 Nil
Base oil
+0.05 MoS2
(CTAB) 1.5:1 6 Nil 30 Nil
Base oil +
0.05% MoS2
(SPAN 80) 1.5:1 5 Nil 32 Nil
Base oil
+0.05 WS2
(CTAB) 3:1 12 5 52 14
Base oil + 0.05% WS2 (SPAN 80) 3:1 14 5 55 15
Base oil
+0.05 MoS2
(CTAB) 3:1 15 8 52 12
Base oil +
0.05% MoS2
(SPAN 80) 3:1 15 7 53 12
Base
oil+0.05
graphene(CT
AB) 1.5:1 4 nil 25 Nil
Base
oil+0.05
graphene(SP
AN 80) 1.5:1 5 Nil 30 nil
[0074] The critical limit of foam produced according to ASTM D 892 is
• At 24oC: Maximum of 10mL after blowing air and nil after allowing to rest.
• At 93.5oC: Maximum of 40mL after blowing air and nil after allowing to rest.
[0075] Based on limits set by ASTM D 892 and Table 2.1, it was observed
that ratio of surfactant to layered nanostructure additives during surface modification of
layered nanostructure additives beyond 1.5:1 increased foaming tendency of the lubricant
significantly. It was also observed that ratio of surfactant to layered nanostructure additives
during surface modification of layered nanostructure additives limited by 1.5:1 did not alter
foaming tendency of lubricant significantly.
EXAMPLE 2.1: KINEMATIC VISCOSITY TEST
[0076] Viscosity of the lubricant is closely related to its ability to reduce friction. Viscosity
index is a parameter that indicates the variation of viscosity with temperature. The effect of
surface modified layered nanostructure additives on the viscosity index of the lubricant was
calculated as per ASTM D 445 standard by measuring visc osity of the layered nanostructure
additive based lubricant at 40oC and 100oC. According to ASTM D 445, a high value
(normally > 90) of the viscosity index indicates that the layered nanostructure additive based
lubricant has good lubricating properties.
[0077] Table 2.2.1 depicts results of kinematic viscosity test for layered nanostructure
additive based lubricant where the lubricant is the SM grade oil. Table 2.2.2 depicts results of
kinematic viscosity test for layered nanostructure additive based lubricant where the lubricant
is CI 4 grade oil.
Table 2.2.1: Results of kinematic viscosity test (SM grade oil)
Sample (SM grade oil: Racer 4 (20W40) Viscosity at
40 C (cSt) Viscosity at
100 C (cSt) Viscosity index
Racer 4 (20W40) 137.18 15.68 119
Racer 4 (20W40)+0.2 % WS2 (CTAB) 144.31 16.28 119
Racer 4 (20W40)+0.2 % 143.28 16.11 118
MoS2 (SPAN 80)
Racer 4 (20W40)+0.2 % 144.22 16.23 119
graphene (CTAB)
Table 2.2.2: Results of kinematic viscosity test (CI 4 grade oil)

Sample (CI 4 grade oil: HP CI 4 (15W40)) Viscosity at
40 C (cSt) Viscosity at
100 C (cSt) Viscosity index
HP CI 4 (15W40) 123.14 14.62 120
HP CI 4 (15W40)+0.2 % WS2 (CTAB) 125.22 14.81 120
HP CI 4 (15W40) +0.2 % MoS2 (SPAN 80) 124.88 14.34 119
HP CI 4 (15W40) +0.2 % graphene (CTAB) 125.34 14.78 120
[0078] As can be seen from Table 2.2.1 and Table 2.2.2, viscosity index of
layered nanostructure additives based lubricants is comparable with viscosity index of
lubricant not comprising the surface modified layered nanostructure additives.
EXAMPLE 2.3: TEST FOR TOTAL ACID NUMBER (TAN)
[0079] Total Acid Number (TAN) is a measure of presence of acids within the nano
suspension lubricant. The Total Acid Number is the amount of potassium hydroxide in
milligrams that is needed to neutralize the acids in one gram of the nano suspension lubricant.
The TAN value indicates potential corrosiveness of the nano suspension lubricant. Thus,
maintaining a low TAN value is essential to maintain and protect components of engines.
Generally, a low TAN value (< 3) gives an indication that the lubricant is non-corrosive.
[0080] Tests were conducted to assess the effect of surface modified layered
nanostructure additives on TAN of lubricants. The table below illustrates the TAN values of
layered nanostructure additive based lubricants prepared using the method of the present
subject matter. Table 2.3.1 depicts TAN of layered nanostructure additive based lubricants
where the lubricant is the SM grade oil. Table 2.3.2 depicts TAN of layered nanostructure
additive based lubricants where the lubricant is the CI 4 grade oil.
Table 2.3.1: Measured TAN (SM grade oil)
Sample (Lubricant Used: SM grade oil-Racer 4) Total Acid number
Racer 4 (20W40) <2
Racer 4 + 0.2 % WS2 (CTAB) <2
Racer 4+0.2 % MoS2 (SPAN 80) <2
Racer 4 +0.2 % graphene (CTAB) <2
Table 2.3.2: Measured TAN (CI 4 grade oil)
[0081] As can be seen from Table 2.3.1 and Table 2.3.2, TAN value of the layered
nanostructure additive based lubricant is comparable with TAN value of lubricant not
comprising the surface modified layered nanostructure additives. Therefore, dispersing the
lubricant with the surface modified layered nanostructure additives does not affect TAN and,
in consequence, is non-corrosive.
EXAMPLE 2.4: TEST FOR TOTAL BASE NUMBER
[0082] Lubricants are required to prevent acidic corrosion within the combustion
chamber of a running engine and should protect different engine components, such as, piston
rings, cylinder liner and piston crown from damage by sulphur or nitrogen containing acids.
Total Base Number (TBN) of the lubricant determines how effectively acids formed during
combustion process of the engine are reduced. The higher the TBN (typically > 5), the more
effective the lubricant is in suspending wear-causing contaminants and reducing the corrosive
effects of acids over an extended period of time.
[0083] The TBN of the layered nanostructure additive based lubricants was tested to
assess the effect of surface modified layered nanostructure additives on the TBN of
lubricants. The TBN was measured by the ASTM D 2896 standard potentiometric titration
with perchloric acid. Table 2.4.1 depicts measured TBN where the lubricant was the SM
grade oil. Table 2.4.2 depicts measured TBN where the lubricant was CI 4 grade oil.
Table 2.4.1: Measured TBN (SM grade oil)
Sample (Lubricant Used: SM grade oil-Racer 4) Total Base number
HP CI 4 oil >10
HP CI 4 +0.2 % MoS2 (CTAB) >10
HP CI 4 +0.2 % WS2 (SPAN 80) >10
HP CI 4 +0.2 % graphene (CTAB) >10
Table 2.4.1: Measured TBN (CI 4 grade oil)
Sample (Lubricant used: SM grade oil-Racer 4) Total Base number
Racer 4 >6
Racer 4+0.2 % WS2 (CTAB) >6

Racer 4+0.2 % MoS2 (SPAN 80) >6
Racer 4 +0.2 % graphene (CTAB) >6
[0084] As can been from Table 2.4.1 and Table 2.4.2, the TBN of layered nanostructure
additive based lubricant is comparable with TBN of lubricant not comprising the surface
modified layered nanostructure additives.
EXAMPLE 2.5: COPPER STRIP CORROSION TEST
[0085] The Copper Strip Corrosion Test is carried out to assess the relative
degree of corrosiveness of a number of petroleum products, including aviation
fuels, automotive gasoline, lubricating oils and other products. In the test, a polished copper
strip is immersed in 30mL of the lubricant at elevated temperature of about 100oC for about 3
hours. After the test period, the copper strip is removed, washed and the color and tarnish
level assessed against the ASTM Copper Strip Corrosion Standard. A classification number
from 1-4 is assigned based on a comparison with the ASTM Copper Strip Corrosion
Standards. A value of 1a denotes excellent protection, 1b denotes good protection, and 1c
denotes sufficient.
[0086] The copper strip corrosion test was performed to assess the effect of surface modified
layered nanostructure additives on the degree of corrosiveness of the lubricant. The lubricant
used for the test was SM 4 grade oil and SM 4 grade oil dispersed with the surface modified
layered nanostructure additives to form the layered nanostructure additive based lubricant.
Table 2.5 depicts results of copper strip corrosion test.
Table 2.5: Results for Copper Strip Corrosion Test
Sample (Lubricant used: SM 4 grade oil-Racer 4) Copper strip corrosion result

Racer 4 1a
Racer 4+ 0.2 % WS2 (CTAB/SPAN 80)) 1a
Racer 4+ 0.2 % MoS2 (CTAB/SPAN 80) 1a
Racer 4+ 0.2 % MoS2 (other surfactants)1b
Racer 4 +0.2 % WS2 (other surfactants) 1b
Racer 4 +0.2 % graphene (CTAB/SPAN 80) 1a
[0087] As can be seen from Table 2.5, layered nanostructure additives surface
modified with CTAB and sodium monooleate (SPAN 80) are better suitable for
automotive environment. Also, it can be observed that layered nanostructure
additive based lubricant dispersed with layered nanostructure additives surface modified with
CTAB and sodium monooleate (SPAN 80) provide corrosion resistance comparable with the
lubricant not comprising the surface modified layered nanostructure additives.
EXAMPLE 3: EVALUATION OF TRIBOLOGICAL PROPERTIES
[0088] In this example, tribological properties of lubricants, such as wear resistance, friction
resistance, and the like, was compared with tribological properties of layered nanostructure
additive based lubricants.
EXAMPLE 3.1: FOUR BALL WEAR TEST
[0089] The Four Ball Wear Test determines the wear protection properties of a lubricant. The
wear tests were conducted for each of petrol engine oil and diesel engine oil as the lubricating
fluid at 40 kgf load and 60 kgf load. The wear tests on gear oils of GL 4 grade were
conducted at 40 kgf and 80 kgf loads. The wear scar diameters (WSD) on the stationary balls
were measured using a Metallurgical microscope. The effect of surface modified layered
nanostructure additives on wear resistance of lubricant was assessed by comparing wear
resistance of the layered nanostructure additive based lubricants with wear resistance of
lubricants not comprising layered nanostructure additives.
[0090] Fig.(s) 3(a)-3(h) illustrate the wear test results for the layered
nanostructure additive based lubricants with the surface modified layered nanostructure
additives dispersed in different lubricating fluids, according to an example implementation.
In the graphs illustrated in the Fig.(s) 3(a)-3(h), the y-axis depicts the wear scar diameter and
the x-axis depicts different compositions of the layered nanostructure additive based lubricant
with different lubricating fluids, such as diesel engine oil, petrol engine oil, and gear oil. The
wear scar diameter is represented in microns.
[0091] The graph 300(a) illustrated in Fig. 3(a) depicts the wear test results of
the layered nanostructure additive based lubricant having diesel engine oil of CI 4 grade as
the lubricating fluid at 40 Kgf load, according to an example implementation. It may be noted
from the graph 300(a) that the wear scar diameter of layered nanostructure additive based
lubricant is lesser than the lubricant not comprising the surface modified layered
nanostructure additives dispersed in it. Addition of surface modified layered nanostructure
additives to the lubricant to obtain the layered nanostructure additive based lubricant reduces
the wear scar diameter substantially.
[0092] The graph 300(b) illustrated in Fig. 3(b) depicts the wear test results of
the layered nanostructure additive based lubricant having diesel engine oil of CI 4 grade as
from the graph 300(b) that the wear scar diameter of layered nanostructure additive based

[0093] The graph 300(c) illustrated in Fig. 3(c) depicts the wear test results of
the layered nanostructure additive based lubricant having petrol engine oil of SM grade as the
lubricating fluid at 40 Kgf load, according to an example implementation. It may be noted
from the graph 300(c) that the wear scar diameter of layered nanostructure additive based
[0094] The graph 300(d) illustrated in Fig. 3(d) depicts the wear test results of
the layered nanostructure additive based lubricant having petrol engine oil of SM grade as the
from the graph 300(d) that the wear scar diameter of layered nanostructure additive
based lubricant is lesser than the lubricant not comprising the surface modified layered
[0095] The graph 300(e) illustrated in Fig. 3(e) depicts the wear test results of
the layered nanostructure additive based lubricant having gear oil SAE 80W90 of GL 4 grade
as the lubricating fluid at 40 Kgf load, according to an example implementation. It may be
noted from the graph 300(e) that the wear scar diameter of layered nanostructure additive

[0096] The graph 300(f) illustrated in Fig. 3(f) depicts the wear test results of the layered
nanostructure additive based lubricant having gear oil SAE 80W90 of GL 4 grade as the
from the graph 300(f) that the wear scar diameter of layered nanostructure additive based
[0097] The wear properties of the layered nanostructure additive based lubricants
having gear oil of GL 4 grade as the lubricating fluid was also tested. The gear oil of GL 4
grade having two different viscosity grades, such as EP 140 and SAE 80 W 90 were used for
the tests. The graph 300(g) illustrated in Fig. 3(g) depicts the wear test results of the layered
nanostructure additive based lubricant having gear oil EP 140 of GL 4 grade as the
from the graph 300(g) that the wear scar diameter of layered nanostructure additive
[0098] The graph 300(h) illustrated in Fig. 3(h) depicts the wear test results of
the layered nanostructure additive based lubricant having gear oil EP 140 of GL 4 grade as
from the graph 300(h) that the wear scar diameter of layered nanostructure additive based
[0099] The Four Ball Wear Test was also used to determine the wear protection
properties of a lubricant with different concentrations of the surface modified layered
nanostructure additives. Different weight concentrations, namely 0.05%, 0.1%, 0.2%, and
0.4% of the layered nanostructure additives of WS2, MoS2, and graphene were taken in base
oil. The wear scar diameter for each concentration was averaged. The average wear scar
diameter for each concentration of the surface modified layered nanostructure additives as
obtained using the Four Ball Wear Test are as shown in Table 3.1.1-Table 3.1.4.
Table 3.1.1: Average wear scar diameter at each concentration of the surface modified
layered nanostructure additives in diesel engine oil CI 4 plus grade engine oil analysis at 40
kgf load
Sample Average wear scar diameter at each concentration of different surface
modified layered nanostructure additives (microns)
Diesel engine oil+0 % surface modified layered nanostructure additives 398.74
Diesel engine oil+0.05 surface modified layered nanostructure additives 397.16
Diesel engine oil+0.1 % surface modified layered nanostructure additives 389.5

Table 3.1.2: Average wear scar diameter at each concentration of the surface
modified layered nanostructure additives in petrol engine oil SM grade engine oil analysis at
40 kgf load
Petrol Engine oil+0% surface modified layered nanostructure additives 389.6
Petrol engine oil+0.05 surface modified layered nanostructure additives 389.43
Petrol engine oil+0.1 % surface modified layered nanostructure additives 370.64
modified layered nanostructure additives in gear oil (GL4 (SAE 80W90))
GL4 (SAE 80W90 ) grade Gear oil analysis at 40 kgf load
Gear oil+0% surface modified layered nanostructure additives 355.95
Gear oil+0.05 surface modified layered nanostructure additives 354.19
Gear oil+0.1 % surface modified layered nanostructure additives 338.9

modified layered nanostructure additives in gear oil (EP 140 GL4)
EP 140 GL4 grade Gear oil analysis at 40 kgf load
Gear oil+0% surface modified layered nanostructure additives 332.59
[00100] From Table 3.1.1-3.1.4, it can be seen that wear scar diameter of
lubricant comprising the surface modified layered nanostructure additives in a weight
concentration in the range of 0.05%-0.2% was lower than wear scar diameter of the lubricant
not comprising the surface modified layered nanostructure additives.
EXAMPLE 3.2: FRICTION TEST
[00101] The friction test was conducted to determine the effect of surface modified
layered nanostructure additives on coefficient of friction of the lubricant. The test was
conducted under the following prescribed test conditions using the ASTM 4 Ball wear tester.
The test was conducted under the following test conditions:

• Temperature 75±2°C
• Speed 600 RPM
• Duration 10 min at each load starting from 10 kgf
• Load 98.1 N (10 kgf) per 10 min increment to a load that indicates
incipient seizure, i.e., sudden increase in friction force value over steady
state on the friction trace.
[00102] The measured coefficient of friction and seizure load are shown in Fig.(s) 4(a)-Fig.
4(h). In the graphs illustrated in the Fig.(s) 4(a), 4(c), 4(e) and 4(g), the y-axis depicts the
measured friction coefficient and the x-axis depicts different compositions of the layered
nanostructure additive based lubricant with different lubricating fluids, such as diesel engine
oil, petrol engine oil, and gear oil. Similarly, in the graphs illustrated in Fig.(s) 4(b), 4(d),
4(f), and 4(h), the y-
axis depicts the seizure load and the x-axis depicts different compositions of the layered
nanostructure additive based lubricant with different lubricating fluids, such as diesel engine
oil, petrol engine oil, and gear oil.
[00103] The graph 400(a) and 400(b) illustrated in Fig. 4(a) and Fig. 4(b) depicts the
friction coefficient and seizure load results of the layered nanostructure additive based
lubricant having diesel engine oil of CI 4 grade as the lubricating fluid, according to an
example implementation. It may be noted from the graph 400(a) that the friction coefficient
of layered nanostructure additive based lubricant is lesser than the lubricant not comprising
the surface modified layered nanostructure additives dispersed in it. Also, it may be noted
from the graph 400(b) that the seizure load of layered nanostructure additive based lubricant
is higher than the lubricant not comprising the surface modified layered nanostructure
additives dispersed in it.
[00104] The graph 400(c) and 400(d) illustrated in Fig. 4(c) and Fig. 4(d) depicts the
lubricant having petrol engine oil of SM grade as the lubricating fluid, according to an
example implementation. It may be noted from the graph 400(c) that the friction coefficient
from the graph 400(d) that the seizure load of layered nanostructure additive based lubricant
[00105] The graph 400(e) and 400(f) illustrated in Fig. 4(e) and Fig. 4(f) depicts the
lubricant having gear oil SAE 80W90 of grade GL 4 as the lubricating fluid, according to an
example implementation. It may be noted from the graph 400(e) that the friction coefficient
the surface modified layered nanostructure additives dispersed in it. Also, it may be
noted from the graph 400(f) that the seizure load of layered nanostructure additive based
lubricant is higher than the lubricant not comprising the surface modified layered
nanostructure additives dispersed in it.
[00106] The graph 400(g) and 400(h) illustrated in Fig. 4(g) and Fig. 4(h) depicts the
lubricant having gear oil EP 140 of grade GL 4 as the lubricating fluid, according to an
example implementation. It may be noted from the graph 400(g) that the friction coefficient
from the graph 400(h) that the seizure load of layered nanostructure additive based lubricant
[00107] From the graphs 400(a)-400(h) it can be seen that addition of the surface
modified layered nanostructure additives to the lubricant decreases the friction coefficient of
the lubricant and increases the seizure load. This indicates that the layered nanostructure
additive based lubricant of the present subject matter provides better anti-friction properties
as compared to the lubricant not comprising the surface modified layered nanostructure
additives.
[00108] Effect of different weight concentrations on the friction coefficient and seizure
load was also studied. Different weight concentrations, namely 0.05%, 0.1%, 0.2%, and 0.4%
of the layered nanostructure additives of WS2, MoS2, and graphene were taken in base oil.
The friction coefficient and seizure load for each concentration was averaged. The average
value of friction coefficient and seizure load for different concentration of the layered
nanostructure additives was as shown in Table 3.2.1-3.2.4
Table 3.2.1: Average friction coefficient and seizure load at each concentration of layered
nanostructure additives in diesel engine oil
Friction coefficien grade oils)t and seizure load of CI 4 plus oils (CI 4 (SAE 15W40)
Sample Avg. seizure load at each concentration Avg. coefficient of friction at
each concentration
Diesel engine oil+0 % surface modified layered nanostructure additives 110 0.0835
Diesel engine oil+0.05 % surface modified layered nanostructure additives 110 0.08153
nanostructure additives in petrol engine oil
Friction coefficient and seizure load of SM grade oils (SM (SAE 15W40) grade oils)
each concentration
Petrol Engine oil+0% surface modified layered nanostructure additives 130 0.099
Petrol Engine oil+0.05% Surface modified layered nanostructure additives 130 0.09763
nanostructure additives in gear oil (GL 4 (SAE 80W90))

Friction coefficient and seizure load of GL 4 (SAE 80W90) oils
each concentration
Gear oil (SAE 80W90)+0% surface modified layered nanostructure additives 130
0.0891
Gear oil (SAE 80W90)+0.05 % Surface modified layered nanostructure additives
186.67 0.0879
Gear oil (SAE 80W90)+0.1 % Surface modified layered nanostructure additives 206.67
0.0854
Gear oil (SAE 80W90)+0.2 % Surface modified layered nanostructure additives 220
0.0725
Gear oil (SAE 80W90)+0.4 % Surface modified layered nanostructure additives 170
0.1097
nanostructure additives in gear oil (GL 4 (EP 140))
Friction coefficient and seizure load of GL 4 (EP 140) oils
each concentration
Gear oil (EP 140)+ 0% surface modified layered nanostructure additives 220 0.0911
Gear oil (EP140)+0.05 % Surface modified layered nanostructure additives 233.33
0.0901
Gear oil (EP140)+0.1 % Surface modified layered nanostructure additives 246.67 0.0834
Gear oil (EP140)+0.2 % Surface modified layered nanostructure additives 273.33 0.0685
Gear oil (EP140)+0.4 % Surface modified layered nanostructure additives 200 0.1163
[00109] From Table 3.2.1-3.2.4 it can be observed that weight concentration of layered
nanostructure additives in the range of 0.05%-0.2% in lubricant provided higher seizure load
and lower friction coefficient than lubricant not comprising the surface modified layered
nanostructure additives.
EXAMPLE 3.4: EVALUATION OF EXTREME PRESSURE PROPERTIES OF GEAR
OILS
[00110] Extreme pressure lubricants, such as gear oils are designed for use in severe
applications across a variety of conditions, including high load, moisture and a wide range of
operating speeds and loads. Thus, effect of surface modified layered nanostructure additives
on extreme pressure (EP) properties of the gear oil as the lubricating fluid was tested.
[00111] In EP test, generally, two parameters, such as Load-wear index and Weld load are
evaluated to determine EP properties. Higher the value of the load wear index and weld load
for a lubricant, the lubricant may be understood to have better EP properties.
[00112] The EP tests were carried out on the layered nanostructure additive based lubricants
and lubricants not comprising the surface modified layered nanostructure additives. Gear oils
of GL4 grade of viscosity grade SAE 80 W 90 and EP 140 were used as the lubricants.
[00113] Fig.(s) 5(a)-5(d) graphically illustrates the variation of extreme pressure (EP)
properties of the layered nanostructure additive based lubricant, according to

an example implementation. In the graphs illustrated in the Fig.(s) 4(a), and 4(c), the y-axis
depicts the load wear index and the x-axis depicts different compositions of the layered
nanostructure additive based lubricant with different gear oils. Similarly, in the graphs
illustrated in Fig.(s) 4(b) and 4(d), the y-axis depicts the weld load and the x-axis depicts
different compositions of the layered nanostructure additive based lubricant with different
gear oils.
[00114] The graph 500(a) and 500(b) illustrated in Fig. 5(a) and Fig. 5(b) depicts the load
wear index and weld load results of the layered nanostructure additive based lubricant having
gear oil SAE 80W90 of grade GL 4 as the lubricating fluid, according to an example
implementation. It may be noted from the graph 500(a) and 500(b) that the load wear index
and weld load of layered nanostructure additive based lubricant is higher than that of the
lubricant not comprising the surface modified layered nanostructure additives dispersed in it.
[00115] The graph 500(c) and 400(c) illustrated in Fig. 5(b) and Fig. 5(c) depicts the load
wear index and weld load results of the layered nanostructure additive based lubricant having
gear oil EP140 of grade GL 4 as the lubricating fluid, according to an example
implementation. It may be noted from the graph 500(c) and 500(d) that the load wear index
and weld load of layered nanostructure additive based lubricant is higher than that of the
lubricant not comprising the surface modified layered nanostructure additives dispersed in it.
[00116] From graphs 500(a), 500(b), 500(c), and 500(d), it can be observed that the load
wear index and weld load is higher in layered nanostructure additive based lubricant
indicating better EP properties.
EXAMPLE 3.5: METALLOGRAPHIC STUDIES ON WORN SURFACE OF BALLS

[00117] To determine the wear characteristics of the layered nanostructure additive based
lubricant, metallographic studies of worn out metallic balls used in the wear test was
performed. The scar area of the worn out metallic balls after the wear test were magnified in a
Scanning Electron Microscope (SEM) and observed for deposition of particles on the worn
out surface of the balls. On viewing the balls in the SEM deposition of the layered
nanostructure additives on the surface of the worn out balls can be seen. Fig. 6 illustrates
characterization of the worn out balls on scanning electron microscope with X-ray diffraction
attachment, according to an example implementation.
[00118] The graph 602 in Fig. 6 depicts the deposition of particles on the worn out balls
when the lubricating fluid, such as gear oil GL 4 grade was used. The graph 604 depicts the
deposition of particles on the worn out balls when the lubricating fluid, such as gear oil of GL
4 grade was mixed with 0.2 weight % of the surface modified WS2 nanoplatelets. The graph
606 depicts the deposition of particles on the worn out balls when the lubricating fluid, such
as gear oil GL 4 grade was mixed with 0.2 weight % of the surface modified MoS2 nano
platelets were used. The y-axis of the graphs 602, 604, and 606 depict the amount of
deposition of the layered nanostructure additives on the worn out balls and the x-axis depicts
the energy of the x-ray radiation used by the SEM. The energy of the x-ray radiation is
represented in Kilo electron volts (Kev). In the graph 604, a peak is seen corresponding to
tungsten (W) and sulphide (S) indicating that surface modified WS2 nanoplatelets were
deposited on the worn surface of the balls and thereby provided wear resistance. Similarly in
the graph of 606, a peak is seen corresponding to molybdenum (Mo) and sulphide (S)
indicating that surface modified MoS2 nanoplatelets were deposited on the worn surface of
the balls and thereby provided wear resistance.
EXAMPLE 3.5: PERFORMANCE TESTING ON A DIESEL ENGINE TEST RIG

[00119] The performance test with lubricating oil was carried out on a diesel engine by
means of a specially designed test rig. The petrol engine test rig consisted of a 1200 cc 4
cylinder, four stroke, turbocharged CRDI diesel engine connected to an eddy current
dynamometer. The specification of the engine used for the performance test is as shown in
Table 3.5.1.
Table 3.5.1: Specification of diesel engine for performance testing
Type 4 Cylinder, 4 stroke, CRDI engine
Ignition microprocessor based engine management
system(ECU),
Displacement 1250 cc
Bore and stroke Bore 69.6 mm, stroke 82 mm
Maximum Power 55 kW @ 4000 rpm
Maximum Torque 190 Nm @ 2500 rpm
Lubricant SAE 15 W40 oil (factory recommended)
[00120] The Morse test is generally used to determine brake power or power available at a
crank shaft of the engine and various efficiencies of an engine. Morse test is carried out at
different speeds and loads to determine various efficiencies of the engine with lubricants.
[00121] Fig. 7 illustrates graphical representations of variations in brake thermal efficiency of
layered nanostructure additive based lubricants in the diesel engine test rig, according to an
example implementation. The graph 700 illustrated in Fig. 7 depicts the variation of brake
thermal efficiency with brake power at 2500 RPM speed of the engine and the graph 702
illustrated in Fig. 7 depicts the variation of brake thermal efficiency with brake power at 4000
RPM speed of the engine. In the graphs 700 and 702 the y-axes depicts the brake thermal
efficiency (ηbrake thermal) and the x-axes depicts the brake power. The brake power is
represented in kilowatts. From the graphs 700 and 702, an improvement in the brake thermal
efficiency at lower as well as higher speeds of the engine is observed with the layered
nanostructure additive based lubricant.
EXAMPLE 3.6: ENDURANCE TEST FOR WEAR AND LIFE OF ENGINE
[00122] The wear performance of layered nanostructure additive based lubricant was
compared to the lubricant not comprising the surface modified layered nanostructure
additives. The wear performance was tested by subjecting the engine lubricated with the
layered nanostructure additive based lubricant to 80 hour test under cyclic loading on a test
rig. The engine test rig consists of a 100 cc single cylinder petrol engine connected to an
alternating current dynamometer. The specification of the engine used for testing wear
performance is as shown in Table 3.6.1.

Table 3.6.1: Specification of engine for testing wear performance
Type Single Cylinder, 4 stroke, Twin spark
Displacement 100cc
Bore x stroke 50mm x 49.5mm
Compression Ratio 8.8:1
Maximum Power 7.8bhp @ 7500 rpm
Maximum Torque 8 Nm @ 4500 rpm
Ignition System Digital Electronic Ignition
Engine Start Electric/Kick
[00123] The alternating current dynamometer was used for loading the engine. The speed of
dynamometer, voltage & current developed by dynamometer, fuel consumption and
temperature of exhaust gases were measured. The cyclic loading was conducted with 16
cycles of 5 hrs cyclic loading. The cyclic loading of 2 ½ hour was done as per the sequence
given in Table 3.6.2.

Table 3.6.2: Sequence of cyclic loading
Test hours Test Conditions
2hr 75% of full load at declared max speed
2hr 100% load at speed to maximum torque
10 min Idling
50 min 100% load at declared max speed.
Test hours Test Conditions
2hr 75% of full load at declared max speed
2hr 100% load at speed to maximum torque
10 min Idling
50 min 100% load at declared max speed.

[00124] After the completion of the endurance test, the engine was dismantled and the
conditions of the aforementioned design features, such as the cylinder liner of the engine and
the piston rings were inspected for possible wear and tear. The wear of the cylinder liner was
measured in terms of increase in diameter of the cylinder liner. The readings of diameter of
the cylinder liner before and after the test were noted down and the difference was reported as
wear loss of the cylinder liner. The wear loss was reported is as shown in Table 3.6.3.
Table 3.6.3: Results of wear of the cylinder liner at different positions of the
cylinder
| | Engine liner wear in \xm |
Lubricant
Position
from
TDC in cm RACER 4 RACER 4+0.2 % WS2 platelets RACER 4+0.2 % MoS2
platelets
2 5.0 4.2 4.33
4 6.5 4.65 4.71
4 7.5 4.66 5.54
8 7.55 3.05 5.81
Mean Wear in |j,m 6.64 4.14 5.18

[00125] Wear of the piston rings in the engine was also determined. The wear of the piston
rings were reported in terms of weight loss of the piston rings. The test results for weight loss
of the piston rings are as shown in Table 3.6.4.
Table 3.6.4: Results for weight loss of the piston rings and gudgeon ring in 80 hr test
Oil RACER 4 RACER 4+0.2 %
WS2
nanoplat elets RACER 4+0.2 %
MoS2
nanoplate lets RACER 4+0.2 % graphene
nano platelets
Piston rings. Serial Weigh t loss mg

Compression ring 1 1IP 2 1 1.1 1.3
Compression ring 1 2IP 18 9.5 11.5 10.8
Expanding ring E1 2 1 1.4 1.5
Oil ring 1 1SR 7 3.5 4.8 4.4
Oil ring 2 2SR 5 1.8 2.4 2.1
Total weight loss, mg 34 16.8 21.2 20.1
Gudgeon pin wear, mg 11 7 8.2 7.2
[00126] From Table 3.6.3 and 3.6.4, it can be observed that the layered nanostructure
additive based lubricant having the surface modified layered nanostructure additives
dispersed therein have substantially reduced the wear in the piston rings and the cylinder
liners of the engine. Thus, the layered nanostructure additive based lubricant of the present
subject matter provide better endurance to the engine than lubricants that do not comprise the
surface modified layered nanostructure additives.
[00127] The fuel consumption was measured during the endurance test at an interval of 2
hours to assess the fuel efficiency of the layered nanostructure additive based lubricant. The
fuel consumption at instant and total fuel consumption were recorded. Fig. 9 graphically
illustrates variation in total fuel consumption for the layered nanostructure additive based
lubricant, according to an example implementation. The y-axis of the graph 800 illustrated in
Fig. 8 depicts the total fuel consumption and the x-axis depicts the time duration of the test.
The time duration is expressed in hours and the total fuel consumption is expressed in Kg/hr.
As may be observed from the graph 800 the fuel consumption with the layered nanostructure
additive based lubricant reduced as compared to the lubricating fluid without having the
surface modified layered nanostructure additives.

[00128] Based on the endurance test it can be observed that the layered nanostructure
additive based lubricants exhibit a reduction in the wear of the components of the engine and
improvement in the mileage of the engine. Further, the stability test, tribological tests, bench
tests, and endurance tests, it can be observed that layered nanostructure additive based
lubricants provide comparable or better results than lubricants not comprising the surface
modified layered nanostructure additives.
[00129] Other embodiments of the present subject matter will be apparent from consideration
of the present specification. It is intended that the present specification and examples be
considered as illustrative only and as encompassing the equivalents thereof.

.
I/We Claim:
1. A method (100) for preparing a lubricant with layered nanostructure additives,
the method (100) comprising:
contacting the layered nanostructure additives with a surfactant and a solvent to obtain a first
mixture;
evaporating the solvent from the first mixture to obtain surface modified layered
nanostructure additives; and
dispersing the surface modified layered nanostructure additives in a lubricating fluid to obtain
the lubricant, wherein the lubricating fluid comprises base oil in a range of 90-99% by weight
of the lubricating fluid and additives in a range of 1-10% by weight of the lubricating fluid,
wherein the weight ratio of the surfactant to the layered nanostructure additives is in a range
of 1.5:1 to 2:1.
2. The method (100) as claimed in claim 1, wherein the layered nanostructure additives
are fabricated from a material selected from the group consisting of transition metal
3. The method (100) as claimed in claim 2, wherein the transition metal disulphides are
selected from the group consisting of molybdenum disulphide, tungsten disulphide, and a
4. The method (100) as claimed in claim 1, wherein the solvent is selected from the
group consisting of hexane, iso-octane, n-heptane, toluene, and combinations thereof.

5. The method (100) as claimed in claim 1, wherein the surfactant is selected from the
group consisting of sorbitan monooleate, cetyl trimethylammonium bromide (CTAB), and a
6. The method (100) as claimed in claim 1, wherein the method comprises sonicating the
first mixture prior to evaporating the solvent.
7. The method (100) as claimed in claim 6, wherein sonicating comprises ultra
sonicating, in an ultrasonic probe sonicator, for a time period of 30 minutes at 50% amplitude
under a pulse mode followed by ultra sonicating for a time period of 30 minutes at 50%
amplitude under a continuous mode.
8. The method (100) as claimed in claim 1, wherein the evaporating comprises stir
heating on a magnetic stirrer.
9. The method (100) as claimed in claim 8, wherein the stir heating is conducted on the
magnetic stirrer at a speed of 500-600 rpm and at a temperature range of 60-70oC.
10. The method (100) as claimed in claim 8, wherein the stir heating provides a dry
powder of the surface modified layered nanostructure additives.
11. The method (100) as claimed in claim 1, wherein dispersing the surface modified
layered nanostructure additives in the lubricating fluid comprises:
adding the surface modified layered nanostructure additives to the lubricating fluid to form a
first suspension; and
sonicating the first suspension to obtain the lubricant.

12. The method (100) as claimed in claim 11, wherein the sonicating the first suspension
comprises ultra sonicating, in an ultrasonic probe sonicator, for a time period of 8-12 minutes
at 50% amplitude under a pulse mode of 0.5 seconds amplitude followed by ultra sonicating
in continuous mode for 30-40 minutes at 50% amplitude.
13. The method (100) as claimed in claim 11, wherein the sonicating the first suspension
comprises ultra sonicating, in an ultrasonic probe sonicator, for a time period of 10 minutes at
50% amplitude under a pulse mode of 0.5 seconds followed by ultra sonicating in continuous
mode for 30 minutes at 50% amplitude.
14. The method (100) as claimed in claim 1, wherein the surface modified layered
nanostructure additive comprises the layered nanostructure additive coated with the
surfactant.
15. The method (100) as claimed in claim 1, wherein the layered nanostructure additives
are selected from the group consisting of nanoplatelets, nanoflowers, and a combination
thereof.
16. A lubricant dispersed with surface modified layered nanostructure additives
comprising:
a lubricating fluid comprising about 90% to 99% base oil and about 1% to 10% additives; and
surface modified layered nanostructure additives from about 0.05 weight % to 0.2 weight %
dispersed in the lubricating fluid, wherein the layered nanostructure additives are selected
from the group consisting of nanoplatelets, nanoflowers, and a combination thereof.

17. The lubricant as claimed in claimed in claim 16, wherein the layered nanostructure
additives are fabricated from a material selected from the group consisting of transition metal
18. The lubricant as claimed in claimed in claim 17, wherein the transition metal
disulphides are selected from the group consisting of molybdenum disulphide, tungsten
disulphide, and a combination thereof.

Nano Additives Based Lubricants

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Nano Additives Based Lubricants

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LUBRICANT WITH LAYERED NANOSTRUCTURE ADDITIVES

to the layered nanostructure additives is in a range of 1.2:1 to 1.5:1.

LUBRICANT WITH LAYERED NANOSTRUCTURE ADDITIVES

HINDUSTAN PETROLEUM Indian Petroleum House, 17, Jamshedji

Maharashtra, 400020, India

3. Preamble to the description

and, in particular, to layered nanostructure additives for lubricants.

introduced between surfaces in mutual contact to reduce friction between them. In

foaming agents, viscosity index improvers, and the like.

[0003] The detailed description is described with reference to the

of illustration, elements in the figures are not necessarily to scale.

[0004] Fig. 1 illustrates

a method for preparing layered nanostructure additive based lubricants, in accordance

with an implementation of the present subject matter.

illustrates HR-SEM images of the layered nanostructure additives, in accordance

with an implementation of the present subject matter.

an implementation of the present subject matter.

an implementation of the present subject matter.

an implementation of the present subject matter.

an implementation of the present subject matter.

load of 40 kgf, in accordance with an implementation of the present subject matter.

lubricating fluid at a load of 80 kgf, in accordance with an implementation of the present

40 kgf, in accordance with an implementation of the present subject matter.

80 kgf, in accordance with an implementation of the present subject matter.

lubricating fluid, in accordance with an implementation of the present subject matter.

lubricating fluid, in accordance with an implementation of the present subject matter.

implementation of the present subject matter.

present subject matter.

the present subject matter.

with an implementation of the present subject matter.

with an implementation of the present subject matter.

accordance with an implementation of the present subject matter.

an implementation of the present subject matter.

[0026] Fig. 6 graphically illustrates characterization of worn out balls using a

implementation of the present subject matter.

nanostructure additive based lubricant, in accordance with an implementation of the present

film lubricants, and forging lubricants.

which comprise of stacks of nanomaterial, predominantly nanosheets. The stacks vary in

resistance to friction and wear and extended lifetime in vacuum.

[0033] Lubricating properties of fully formulated lubricating fluids may be enhanced by

dispersing these layered nanostructure additives, such as nanoplatelets and nanoflowers, in

modifying effects which make them suitable for use as lubricants.

cause shearing of the stacks in the layered nanostructure further

leading to destabilization of the nanostructures in the lubricating fluid. Therefore, the

which does not agglomerate or settle over an extended period of time.

additives is in a range of 1.2:1 to 1.5:1.

also shows improved performance characteristics, such as anti-wear, anti-friction, and

extreme pressure characteristics when compared to lubricants without the layered

nanostructure additives can be dispersed in a stable manner in lubricating fluids comprising

present subject matter to the description and figures illustrated herein.

nanostructure additives, in accordance with an implementation of the present subject matter.

properties, as will be explained later. Layered nanostructure additives having greater

to steric repulsion between the surfactant molecules attached to the surface of

the nanostructures, thereby

group consisting of sorbitan monooleate (SPAN 80), cetyl trimethylammonium bromide

foaming tendency of the lubricant, as will be explained later. In one implementation, a

form the first mixture.

bonding of the surfactants to the layered nanostructure additives. In an example

nanostructure additives, thereby increasing stability of layered nanostructure additives in the

superficially modifies the surface of the layered nanostructure additives

by one of chemisorption and functionalization, thereby increasing lipophilicity of the

packed and stored or dispersed in the fully formulated lubricating fluid.

which form during a combustion process in an engine, a friction-reducer and anti-oxidant,