A UNIQUE SHEAR CAPTIVE GREASE FOR HIGH END APPLICATIONS

Nidhi Jain, S C Nagar, Dr E Sayanna & Sudhir Sachdeva

M/s. Siddharth Grease & Lubes Pvt. Ltd.
Plot No. 13, Sector-3, IMT Manesar
Haryana-122050 (India)
ABSTRACT:

Consistency of a lubricating grease would change if it is subjected to mechanical shear

in any suitable device. The ability of the greases to maintain its consistency under
mechanical shear is called shear stability or mechanical stability. Working Stability (ASTM
D217) and Roll Stability (ASTM D1831) are the two standard test methods that are widely
referred for checking shear stability of lubricating greases. Roll stability test appears to
be more significant compared to mechanical stability test as the shearing action in bearing
races is nearly identical to rolling. Lower the change in consistency the better is the
product considered in shear stability.

The standard roll stability test depicts the change in grease consistency at ambient
temperatures after two hours. Many grease developers modify the standard test method
by a lot of variations in the test temperature and duration. Normal operating temperature
of bearing is in the range of 80oC while under the extreme conditions the bearing
temperature may go further high. It is anticipated that greases may further excel in
performance if lower values in both mechanical and roll stability tests are obtained.

Many functional polymer suppliers claim improved performance in mechanical stability

and roll stability tests at ambient temperatures but in the present paper we aimed to
improve the performance by altering the chemistry of thickener not by doping any
polymer.

Based on the industry requirement, we at Siddharth Grease & Lubes Pvt Ltd have
developed “A New Shear Stable Grease Using No Polymer” having excellent
mechanical and roll stability even at elevated temperatures. The new greases have been
extensively evaluated for life in FAG FE9 & HTWB Life Tester. Important properties of the
newly developed grease like dropping point, mechanical stability, and roll stability at
ambient and elevated temperatures even on increasing test duration and are discussed
in this paper.
Key Words: Shear Stability, Roll Stability, FAG FE9 test, HT WB Life Test, polymers.

INTRODUCTION:

A grease consists of a physical matrix containing a fluid base oil, a thickener which
provides its gel structure. When a grease is worked (subjected to mechanical stresses),
its consistency or hardness will change. The reason for the change is that the soap fibers
are being modified by the mechanical actions. In general, a grease will soften or become
more fluid when worked. If a grease softens when worked it is referred to as thixotropic;
however, if the grease hardens, it is called rheopectic. A good grease must have good
shear stability implying that it exhibits a little change in penetration after undergoing
mechanical stress (1). Mechanical stability is an essential performance characteristic of
lubricating grease as it is a measure of how the grease consistency will change in service
when it is subjected to mechanical stress (shear) resulting from the churning action
caused by moving elements or vibrations generated by, or external to, the application
(2&5). Excessive grease softening in a bearing may eventually cause grease to leak out
from the housing, requiring more maintenance and frequent grease replenishment to
avoid premature failure resulting from lack of lubricant in the rolling elements. Shear
stability varies from grease to grease. A grease with poor mechanical stability is not
preferable because it may experience large changes in consistency that can cause a
grease to leave its optimal operation range after being semifluid and allow an element to
fail. The soap used as thickener plays the major role in grease stability. To have good
mechanical stability, greases are developed through careful selection of the thickener
composition and optimization of the manufacturing process. Though mechanical stability
test as per ASTM D217 depicts if a grease show <40 units change in 100,000 strokes, it
is rated as good.

Another test is Roll Stability which holds equal significance to evaluate shear stability of
greases. The test is normally conducted at room temperature for two hours as per
standard ASTM D1831 test, but the specification designers have made the test conditions
more stringent by varying the standard test conditions like increase in operating
temperature from ambient to 800C, conducting test in presence of water and enhancing
duration of test. Due to the fibre instability of the thickener above 60°C, considerable
shortening of the thickener fibres and increasing penetration values after shearing of the
grease in a roll stability tester at 75°C, as well as transformation from shear thinning to shear
thickening at the shear rate of 1800 s−1 and 80°C, were observed (3).

In real field application and use, ingress of environmental contaminants sometimes is

unfortunately a common reality which often adversely affects the mechanical stability of
the greases. It is important that grease not only be developed to provide excellent
structural stability in a perfect state, but also in the presence of environmental
contaminants such as water, process fluids, or other contaminants. This can be assessed
by means of laboratory bench tests operating in a variety of conditions with presence of
water (4). In order to bring the above environmental contaminants into tests conditions
researchers try to conduct mechanical and roll stability in presence 5-10% of water and
is considered OK if the structure is not much deteriorated indicating that the thickener is
capable of sustaining stress and strain. Thus, a good grease must also be capable of
depicting low to moderate changes in terms of penetration if the above tests are
conducted in presence of water.

EXPERIMENTATION:
Four batches (A-D) were prepared using different thickener chemistries initiating
development work from simple lithium base to Li-Ca then further shifting over to Li-
complex doping different complexing agents like boric acid and di-basic acids using VG
150 base oil. All these batches were evaluated for mechanical stability and roll stability at
80oC for 50 hrs. Test data is indicated in Table-1.
 Candidate Type
A Lithium Grease in VG 150
B Li-Ca Grease in VG 150
C LC Grease with Boric Acid as complexing agent in VG 150
D LC Grease with Azelaic acid as complexing Agent in VG 150
E Li Grease with (ASSCT) technology
F LC EP Grease with (ASSCT) technology

Table-1 : Mechanical Stability & Roll Stability Test Data

Candidate Type Mechanical Roll Stability

Stability 105 X
Penetration Change
Room 80oC
Temp, 2 50 Hrs
Hrs.
A Lithium Grease in VG 150 +30 102
B Li-Ca Grease in VG 150 +22 +18 85
C LC Grease with boric acid +27 68
as complexing agent in VG
150
D LC Grease with Azelaic +29 62
as complexing agent in VG
150

DEVELOPMENT OF SHEAR STABLE GREASE:

Mixed soap greases were initially developed to improve the short comings of individual
simple soap-based greases. The most preferred thickener choice is mixed
soap grease i.e., lithium-calcium as lithium improves the high temperature resistance
of the resulting grease while the calcium explores the possibility of developing a grease
having better mechanical stability and roll stability. Work was initiated in different direction
using our own Advanced Soap Salt Complex Technology (ASSCT) on Li thickener
chemistry. This approach was having limitation in dropping point around 208oC. The
grease E was finally evaluated, and the test results are shown in Table-2. The developed
product was tested extensively in mechanical stability up to 5 X 105 strokes (Table-3).
Similarly Roll Stability test was studied at ambient and elevated temperatures with
increased test duration (Table-4 & 5). To further improve dropping point further
complexing of thickener was done and could achieve DP > 260 oC. Based on best results
obtained on a candidate batch dosage of dibasic acid was further optimized to meet other
characteristics also. After observing repeated improvements in test results manufacturing
process was finally optimized based on better results and yield. Additive studies were
also carried out after evaluation of base greases. Finally, a wonderful product has been
developed which was completely evaluated for various characteristics (Table-6) and
christened the grease as Wonder Grease.
PERFORMANCE TEST:
FAG FE8 & FE9 tests are mainly used to evaluate the friction & wear characteristics of
rolling element bearing. It can simulate different operating conditions, and the test results
can be used to simulate the practical application of bearing, and study the friction of
grease, lubrication, rolling bearing material under different working conditions.

FE 9 TEST: DIN 51821

The test rig with its test units is intended exclusively for examining the service life of
grease in Angular Contact Ball Bearings.
Angular contact ball bearings type FAG Z-No. 529689 are installed in the 5 units of the
test rig. They are loaded axially with a force of F = 1.5/3/4.5 kN and are operated at the
specified test -1 speed of n = 3000/6000 min. The required temperature of q = 120 - 200°C
is achieved by means of the resistance heating unit. The test is continued until the
bearings require at least the double steady-state moment for operation due to insufficient
lubricity of the grease.
The FAG FE9 test as per DIN 51821 uses five angular ball bearings, rotating at 6000 rpm,
under an axial load (usually 1500N). Test temperature is selected (120 to 200 oC), and
time to failure is based on a two-fold increase in the power requirement to rotate the
bearing. The times at which the bearings have a failure probability of 10% and 50%
(denoted by L10 and L50) are calculated from the data by using Weibull analysis. This
method is the basis for upper operating temperature claims in the DIN (Deutsches Institut
für Normung) 51825 grease classification system.
The Greases E& F were extensively evaluated for life tests at some renowned overseas
independent laboratories.
RESULTS & DISCUSSION:

It is a well-known fact that >80% of the bearings are lubricated with greases, though the
percentage of greases is <5. Mechanical stability & roll stability are of immense
importance when dealing with the long-term service-length of grease-lubricated bearings.
Poor stability will lead to consistency degradation of the grease, because of mechanical
forces between the rolling parts of the bearing. Higher change in penetration numbers
either in working or in rolling show greater grease thinning and, therefore, less stability.
Leakage of grease through seals, or at worst a total failure of the bearing may be
experienced in operation. Similarly, if roll stability at elevated temperature is good, grease
will not lose its structure and can work consistently resulting in increased life of bearings.

The test data of mechanical stability and roll stability of developed grease with a dropping
point of 208 C is indicated in Tables 1-4 clearly depict that the product is excellent in both
mechanical stability and roll stability. This newly developed grease has shown +20 units
change in 1 Lakh strokes and 30-34 units’ changes in 2 to 5 Lakhs strokes working
indicating that grease is not undergoing mechanical degradation even after 5 lakhs double
strokes. Similar trend is visible in roll stability at ambient and in elevated roll stability test.
Change in penetration is very abysmal i.e., 12 to 25 units even after prolonged rolling at
80oC These two properties have contributed to achieve long life of 130 hrs in High
Temperature Wheel Bearing (HTWB) Life test as per ASTM D3527. Though test data has
been generated on grease made with 150 cSt base oil at 40 oC, however, product with
higher base oil viscosities have also been designed and evaluated.

Another semi-synthetic product was developed in higher viscosity base oil using the
above similar chemistry, but the thickener molecule was further complexed to boost the
dropping point around 262oC.The EP, AW, AO and other additives were also incorporated
into the developed grease. Tests data has been given in Table-5. Besides physio
chemical tests, test data of roll stability at different temperatures like ambient, 50 & 100 oC
is having similar trend with little change in penetration number in working and that too on
prolonged rolling. Both the working stabilities have shown a quantum jump of 390 hrs in
ASTM D3527 HTWB life test. Based on the tests data indicated in Table-5, it is evident
that the grease is expected to perform exceptionally good in field.

The grease E was also tested for FE 8 TEST and passes the test. This product is
commercialised by one reputed company and is being supplied regularly.
The grease F was tested for FE 9 TEST at 140 & 160oC.

Recommended Applications:
Based on the extraordinary life tests data, we embarked upon field trials of this grease in
long life applications. The grease has shown promising results in the field for 300K
mileage and is being evaluated for 500K and EV application also. It has also found to be
a problem solver for many critical industrial applications, where good high temperature
stay put property is required. This grease can be true high-performance grease for
important industrial applications, where no unwanted breakdowns are warranted. Based
on the evaluation data obtained in FE 8 & FE 9 TEST Rigs including HTWB Life tester,
we strongly recommend the developed products in the following applications:

• Greases for heavy duty automobiles for long GDI.

• Railroad Greases
• Electrical Vehicles
• Critical Steel Plant & other critical areas.

References:

(1) https://tribologynews.wordpress.com/2009/05/28/grease-mechanical-stability/
(2) Tribology International Volume 33, Issues 3–4, April 2000, Pages 217-223
(3) https://pubs.rsc.org/-/content/articlelanding/2016/ra/c5ra20288d/unauth#!divAbstract
(4) https://www.ispatguru.com/grease-and-grease-lubrication
(5) https://evolution.skf.com/testing-times-for-greases/
(6) A new method for determining the mechanical stability of lubricating greases
Tribology International 33(3-4):217-223, April 2000

Table-2 : GREASE E
S. No. Test Parameter Test Method Test Results
1 Penetration, Worked 60X ASTM D 217 245
Change in penetration after 105X +20
2 Dropping Point, oC ASTM D 2265 208
3 Copper Corrosion at 1000C, Rating ASTM D 4048 1b
4 Base Oil KV 40oC, cSt Formula 150
5 Roll Stability ,80 oC ,50 Hrs., ASTM D 1831
Change in penetration + 20
6 WB Life ASTM D 3527 130 Hrs
7 Low Temp Torque, Nm IP 186
At -10oC 0.04/0.02
At -20oC 0.12/0.07
8 Heat Stability, % wt. ASTM D 6184 0.90

The above developed grease was extensively studied for extended mechanical stability
for 1X 105X; 2 X105X; 3 X105X; 4 X105X and 5 X105X. The test data of mechanical working
are indicated in the Table (III)

Table-3
S. No Test Parameter Test Method Test Results
1 Penetration, Worked 60X ASTM D 217 245
Change in penetration after 1x 105X +20
Change in penetration after 2x 105X +30
Change in penetration after 3x 105X + 32
Change in penetration after 4x 105X + 33
Change in penetration after 5x 105X + 34
The developed grease was studied for roll stability at ambient temperature for 2 hrs and
16 hrs. The test data of roll stability are indicated in the Table (III).

Table-4
1 Roll Stability at ambient temperature ASTM D 1831
Change in penetration after 2 Hrs. -10
Change in penetration after 16 Hrs. +9

Table-5
1 Roll Stability ,80oC
Change in penetration after 24 Hrs. +12
Change in penetration after 50 Hrs. ASTM D 1831 +20
Change in penetration after 100 Hrs. (Modified) +25
Change in penetration after 150 Hrs. +23
Table-6
GREASE F
S. No Test Parameters Test Method Test Results
1 Colour - Brown
3 VI ASTM D2270 110
4 Thickener Type - Proprietary
5 Base oil viscosity at 100oC in cSt ASTM D445 18.5
6 Worked Penetration (1/10 mm) at 25˚C
60 Double strokes ASTM D217 284
100,000 Double strokes (+18)
7 Drop Point, ˚C ASTM D566 262
8 Shell 4 ball OK Load, kgf ASTM D2596 315
9 Four ball wear scar diameter, mm ASTM D2266 0.52
10 Fretting Wear, mg ASTM D4170 8
Roll Stability, change in penetration- a) + 14
a) For 2 h at room temperature ASTM D1831 b) + 16
b) For 16 h at 50 ˚C c) + 15
d) For 100 hrs at 100
12 Water washout, % mass ASTM D1264 1.9
13 Oil separation during storage, % mass ASTM D1742 1.4
14 Oxidation Stability. Pressure drop at 100 h ASTM D942
,100oC, Drop in pressure in psi 1.5
15 Rust preventive properties ASTM D 1743 Pass
16 EMCOR Test (DW) ASTM D 6138 0,0
17 Copper Corrosion ASTM D 4048 1a
18 1). 0.80 g
2). No deposits in
the WB races &
ASTM D1263 rollers no abnormal
changes in
WB Leakage Test, consistency or
1) Leakage in mass, g structure of the
2) Other observations material indication of
dry running of races
19 High temperature wheel bearing life test ASTM D 3527 390
20 FAG FE 9 (h),6000 rpm/1500N
a) 120 oC Actual data given in
b) 140 oC presentation
c) 160 oC