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1 Tribological Behaviour of Neem Oil with and without Graphene

2 Nanoplatelets using Four Ball Tester

3 B. Suresha,1 G. Hemanth,1 Apurva Rakesh1 and K. M. Adarsh1


1
4 Department of Mechanical Engineering, The National Institute of Engineering, Mysore
5 570008, India

6 Correspondence should be addressed to Suresha B; sureshab@nie.ac.in

7 Abstract
8 This research work aims to study the behaviour of Graphene nanoplatelets (GNPs) under wear
9 preventive and extreme pressure condition as an anti-weld additive for neem oil. The effect of
10 the neem oil blended with various loading of GNPs on the friction and wear characteristics has
11 been investigated. Further, it has been found that 1 wt% of GNPs with neem oil bio-lubricant
12 gives lowest coefficient of friction and smoother wear scar as noticed from the optical
13 micrographs. The extreme pressure test was performed on neem oils with GNP additives. The
14 extreme pressure test results indicated the improvement in seizure load of neem oil by 27.8%
15 at 0.5 wt. % of GNPs in relation to pure neem oil. Optical microscopy of wear surface revealed
16 the adhesive wear and the formation of wedge cutting edge in GNPs modified neem oil.

17 1. Introduction

18 The friction and wear characteristics of machine components is a significant research area that
19 is being thoroughly studied. A lubricant, apart from being used in automobiles, finds its
20 necessity in pneumatic circuits, food processing machinery, airplanes, hydraulic press and
21 hydraulic jacks [1-3]. The operating conditions to which lubricants are exposed dictates its
22 grade and shelf life. There are many researchers studied to improve the properties of lubricant
23 and reduce the material loss caused to the machine components [4, 5]. Continuous efforts have
24 been made to develop technology to avoid ill effects on environment [6]. The rate of
25 biodegradability of mineral oils is around 30-65% whereas, bio-based substitute is having
26 almost 95% [7]. Erhan et al. studied that around half a cent of oils used as lubricant reaches out
27 to the atmosphere by as spillage, evaporation, and leakage [8].

28 Owing to the ill effects of mineral and synthetic oils on environment and human health and
29 increasing oil demand and prices, the research objective was framed to pursue research on bio
30 resources in late 90s and early 21st century [9-11]. Regular efforts were made to substitute
31 mineral oils with bio-based oils namely jathropa, spirulina, pongamia [12-14]. Friction and
32 wear of tribo system depends on various tribo parameters like load, velocity, sliding distance
33 and type of lubrication. Hsu et al. concluded that the effect of hydrodynamic conditions of
34 lubricant does not have a significant effect on surface wear. However interaction between
35 lubricant and surfaces in contact influences the tribo properties [15]. The bio oils have superior
36 anti corrosive, high flash point and fire point, feeble aquatic toxicity. Lubricants extracted from
37 edible oil seeds pose severe food versus fuel issues which can be overcome by non-edible oils
38 [16]. Hence a lot of focus is upon non-edible oils mentioned above. Many researchers have
39 studied the friction and wear behaviour of bio-based oils [17-19]. The bio oils comprise of
40 triglycerol, and polar nature of the fatty acids allow it to form bond with metallic surfaces and
41 create a thin mono layer that is beneficial in reducing wear and friction [18, 19]. The bio based
42 oils have a few short comings, like poor thermal oxidative stability, non-negative pour points
43 and gumming effects [20-23].

44 Incorporation of nano-fillers into the oil has shown a lower coefficient of friction and a
45 smoother wear scar. The reduction in wear is attributed to an increase in the viscosity of the oil
46 [24]. The viscosity enhancement was associated with the number of particles available per unit
47 volume of oil. There are a lot of parameters that dictate the behaviour of nanoparticles in the
48 lubricant, some of which are size, geometry and chemo-physical properties. Nanoparticles tend
49 to diffuse between two mating components thereby avoiding metal contacts leading to wear
50 reduction. Some nano additives form a bond with metal surfaces while some convert sliding
51 into rolling friction [25-27]. Masuda et al. proved the incompatibility of metallic nano-fillers
52 with lubricant and concluded that surface activity is responsible for this incompatibility [28].
53 Not only the particulate additives play a role in enhancing the tribo properties, blending bio-
54 based oils into lubricant also showed multi-functional behaviour [29-32]. Li et al. has illustrated
55 the application of natural garlic oil as a high performance extreme pressure additives for
56 lubricants [33]. Ossia et al. have affirmed the presence of eicosanoic and octadecanoic acids in
57 castor and jojoba oil and enhancing their oxidation stability and tribological properties [34].
58 Carboneceous particles like soot, graphene, multiwalled carbon nanotube showed very good
59 lubricity [35-37].

60 Neem is a native tree to Indian-subcontinent and is widely grown in Indian states namely, Uttar
61 Pradesh, Tamilnadu and Karnataka. Its applications are discussed in ayurvedic literature.
62 Schmutterer has analysed the effect of neem derived product as a pesticides [38]. Subbalakshmi
63 et al. has discussed about usage of neem as fertilizers, soil conditioner fumigant, pesticide etc
64 [39]. Sanuja et al. has discussed neem oil based bio composite for food packing application
65 [40]. Neem oil is found to have a significant role in the medical field [41-44]. Nentwig studied
66 the behaviour of neem oil as repellent [45]. Chaudhari et al. has discussed a self-healing coating
67 of Polyurethane prepared from neem oil polyesteramides [46]. Hence, the present research
68 investigates the role of graphene nanoplatelets on viscosity, friction and wear as well as on
69 seizure load which are important factors which are accounted for correct selection of the
70 required lubricant in different moving components of food processing machines. Hence neem
71 oil was preferred for the further conscientious investigation with and without grapheme
72 nanoplatelets.

73 2. Materials and Methods


74 Neem oil (NO) were procured from NIE-Center for Renewable Energy and Sustained
75 Technology, Mysore, India. The Gra2phene nanoplatelets (GNPs) was procured from Sigma
76 Aldrich, Bangalore, India. The specifications of GNPs are, surface area 750 m2/g, the GNPs
77 considered is structured out of 3-6 layers of <50 nm thick. The density of the material is 2.0-
78 2.25 g/cm3. Figure 1(a) shows the Transmission Electron Microscopic image of GNPs obtained
79 from product data sheet [47]. It can be observed from TEM image that the GNPs are semi-
80 transparent and they are in order of few nanometres. Figure 1 (b) shows the XRD pattern of
81 GNPs [47].
82

83
84 FIGURE 1: (a) Transmission electron microscopic image of GNPs with 200 nm scale bar, (b) XRD pattern of
85 750 m2 GNPs [47].

86 2.1.Extraction of Oil

87 The neem oil was produced from its seeds. The oilseeds were cleaned and crushed to extract
88 oil out of it. The oils so obtained were filtered in two stages. Firstly, with a coarse filter of 180-
89 micron mesh sieve and later with 50-micron mesh sieve to remove finer impurities. Some of
90 the particulate impurities were settled at the bottom of the container which was later discarded.

91 2.2.Blending Oil with Graphene Nanoplatelets

92 The oil obtained was ultrasonicated with GNPs. The loading of nanofillers has a great effect of
93 the functionality of bio oils as lubricants with about 0.1 to 1.5 wt. % stated as the optimum
94 loading for nanofillers in majority research works carried out [48-50]. Therefore, in the present
95 work, for the purpose of evaluating the effect of GNPs loading on the tribological properties
96 of neem oil, nano-lubricants have been made at four different loadings of 0.25, 0.5, 0.75, and
97 1.0 wt. % by incorporating GNPs to neem oil. The ultrasonication was performed for 15 min
98 at a frequency of 22 kHz using Johnson Ultrasonicator. Figure 2. shows the process chart of
99 the current research.

100
101 FIGURE 2: Work process chart of the current experimental work.

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102 2.3.Measurement of Viscosity

103 The viscosity of the blended oils was tested along with bio-based oils. The viscosity test was
104 carried on the redwood viscometer whose test procedure is governed by IP 70/62. 50 cm3 of
105 oil is allowed to flown down and corresponding flow time was recorded for the further
106 calculations. The orifice diameter is 1.62mm. The test was initiated at 30°C and for every 5°C
107 rise in temperature, the consecutive reading was noted. Five trials were done to affirm the
108 values. Figure 3 shows the schematic representation of Redwood viscometer. The equation 1
109 was used to evaluate kinematic viscosity.
𝟎.𝟔𝟓
110 𝝑 = 𝟎. 𝟎𝟎𝟐𝟒𝟕 × 𝒕 − (1)
𝒕
111

112
113 FIGURE 3: Sectional front view of the Redwood viscometer.

114 2.4.Friction and Wear Test

115 The wear preventive characteristics of the NO-GNPs based lubricant is examined under four
116 ball tribometer. The test procedure is governed by ASTM D 4172 [51]. The tribometer was
117 procured from Magnum Engineers, Bangalore, India. The chromium steel balls of 12.7 mm
118 diameter and 64-66 HRC with mirror polished surface was used for the investigation. The test
119 duration is 60 minutes, the temperature of the oil is 75°C and the rotation speed was kept
120 1200±1 rpm. Test load was maintained to be constant, that is 40±0.1 kg. The coefficient of
121 friction and wear scar diameter was obtained. Figure 4 and Figure 5 shows the four-ball tester
122 setup.
123 The extreme pressure test was performed according to ASTM D2783 standard [52]. The test
124 started from 400N with an increment of 100N till the first weld was observed. Later the load
125 was decreased by 20N for each trial until the seizure load is obtained. Five trials were
126 performed as mentioned above to affirm the values. The test conditions are as follows, variable
127 load, speed was maintained to be 1760±30 rpm, oil temperature was 25°C and the duration of
128 the test was 10 seconds.

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FIGURE 4: Schematic diagram of the four ball tester. FIGURE 5: Assembly of four ball tester with ball
holder cup.
129
130 3. Results and Discussion
131 3.1.Effect of GNPs Loading on Viscosity of Neem oil
132 TABLE 1: Measured kinematic viscosity of various wt. % of GNPs-Neem nano-lubricants.

Kinematic Viscosity at 40°C


Nano-lubricant formulations Designation
(mm2/s)
Pure neem oil NO 53.3 ± 0.35
Neem oil mixed with 0.25 wt. % 0.25% GNPs-NO 55.5 ± 0.61
GNPs
Neem oil mixed with 0.50 wt. % 0. 50% GNPs-NO 58.7 ± 0.19
GNPs
Neem oil mixed with 0.75 wt. % 0.75% GNPs-NO 62.3 ± 0.53
GNPs
Neem oil mixed with1.0 wt. % GNPs 1.0% GNPs-NO 67.193±0.4
133
134 The rate of fluid resistance against it’s flow is called viscosity, which is one of the vital factor
135 for selecting a suitable lubricating oil for moving components in machinery. Since one of the
136 important properties of a lubricant is viscosity, in the present research work, the focus is on
137 effect of loading of GNPs into the neem oil which results in the change of viscosity. For this
138 reason, viscosity of the lubricating oil which did not contain nanoparticles considered as a base
139 fluid (neem oil) and also viscosity of the bio-lubricants which contain GNPs at four loadings
140 0.25, 0.5. 0.75, and 1.0 wt. % and with increase in temperature from 30°C to 55°C was
141 measured. The experimental results are summarized in Table 1 and also shown in Figure 6. As
142 it can be seen, the viscosity of GNPs-NO nano-lubricants from 30°C to 55°C temperatures had
143 increased by increasing the loading of GNPs, although the rate of changes in viscosity at lower
144 loadings is much smaller than that at higher loadings.
145 The exciting point related to the amplified viscosity of GNPs-NO nano-lubricants with 1.0 wt.
146 % loading is that for increasing temperatures, the viscosity of the neem oil without GNPs had
147 a significant amount of decrease. When GNPs are incorporated to the neem oil, they are
148 positioned between the neem oil layers and escort to ease of fluid layer movement on each
149 other. As a result, the viscosity will decrease slightly and the decreasing trend can be seen for
150 0.25 and 0.5 wt. % GNPs-NO nano-lubricants as shown in Fig. 6. As GNPs loading increases,
151 nanofillers agglomerate and create bigger and asymmetric particles, which prevent movement
152 of fluid layers on each other; hence the viscosity increased for higher loadings (0.75 and 1.0
153 wt. %) of GNPs-NO nano-lubricants. The same behaviour was observed by other researchers

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154 with different liquids and nano additives [53-56]. Wang et al. observed about 86% of
155 improvement in the viscosity of distilled water upon the incorporation of Al2O3 [53].
156

157
158 FIGURE 6: Measured kinematic viscosity of GNPs-Neem nano-lubricant for various wt. % with temperature.
159
160 3.2.Wear Preventive Characteristics GNPs Modified Neem oil
161 The wear preventive characteristics were first conducted on pure NO and then followed by
162 blended oils of NO. There are many factors that influence the lubricant properties. In this
163 regards, the coefficient of friction versus oil combinations plot is as shown in figure 7. It is
164 seen that the coefficient of friction is reduced by 7.5 % on incorporation of 0.25% GNPs-NO,
165 25.2 % with 0.5% GNPs-NO, 28.9 % with 0.75% GNPs-NO and the highest reduction was
166 found with 1.0% GNPs-NO which is around 41.4 % with the base NO. A significant reduction
167 of 23% was observed in wear scar diameter with 1.0% GNPs-NO in relation to unblended NO.
168 This reduction is associated with an increment in the viscosity of the oil which helps in the
169 formation of thin film owing the decrease in wear scar diameter as well.
170 From the Figure 8, it can be observed that GNPs modified oil with lower percentages of GNPs
171 showed darker concentric grooves which depicts abrasive wear whereas in higher percentages
172 of GNPs showed adhesive wear. It is these grooves which are responsible for holding GNPs
173 back on the wear surface causing the reduction in wear, the same phenomenon was discussed
174 by Huang et al. where they have incorporated graphite sheets [57].
175 The load is the primary characteristics that affect the wear. Ing et al. proved that variations in
176 the load largely dictates the wear on the surface of the steel balls [58]. The chemical
177 composition of the lubricant oil affects the wear preventive characteristics. Stachowiak and
178 Batchelor has discussed that synthetically produced lubricants have compounds containing
179 phosphides and sulphide ions which have a tendency to react with the surface of the steel balls
180 which prevent the metallic contact to a certain extent and reduce the wear [59]. However, the
181 sulphide and phosphide compounds are not present in bio-based resources which makes the
182 bio-based resources to have higher wear scar than mineral or synthetic oils [58]. The reason
183 for the improvement in anti-frictional properties is the enhancement in viscosity whereas,
184 improvement in the anti-wear property is due to the uniformity in the dispersion of GNPs. The
185 quintessential proof for the latter condition can be found in the work of Hu et al. [60].

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186
187 FIGURE 7: Mean coefficient of friction of various wt. % of GNPs-Neem nano-lubricants.

188
189 FIGURE 8: Optical micrographs of wear scar diameter: (a) pure neem oil, (b) 0.25 wt. % GNPs-neem oil, (c)
190 0.50 wt. % GNPs-neem oil, (d) 0.75 wt. % GNPs-neem oil, (e) 1.0 wt. % GNPs-neem oil.

191 3.3.Effect of GNPs modified Neem Oil on Extreme Pressure Characteristics

192 The extreme pressure test was started with NO to seek for their seizure load followed by the
193 blended oils. The GNPs blended into oil will help to sustain the failure by enhancing the seizure
194 load. Apparently, increment in viscosity is associated with the enhancement in seizure load.
195 Upon increase in viscosity, thin film is formed, the load carrying capacity also increases and
196 thereby seizure can be adjourned. It is observed from figure 9 that seizure load was found to
197 be increased with all combinations of GNPs blend. Among all combinations of oils 0.5%
198 GNPs-NO has portrayed the outstanding improvement in seizure load of 2300 N owing to
199 27.7% increment in seizure load in accordance with NO. However the higher percentages of
200 GNPs modified NO didn’t show the further increment in seizure load.
201 Binu et al. have discussed the relation between the viscosity and load carrying capacity by
202 using different models and experimental validation [61]. There is a correlation between the
203 minimum oil film thickness and a viscosity [62]. The viscosity improves load carrying capacity

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204 [63]. Hence it can be said that the load on the component controls the minimum oil film
205 generation. Though the increment in viscosity was found converting sliding into abrasive wear
206 finally welded the balls to one another converting abrasive wear to adhesive wear.
207

208
209 FIGURE 9: Seizure load of various wt. % of GNPs-Neem nano-lubricants.
210 Kozma M discussed in his work about the relation between the scuffing load and viscosity and
211 found that with increment in viscosity scuffing load will increase up to a certain extent and
212 then remains constant with increase in viscosity [64]. However, there is a limitation to the
213 extent to which nanoparticles can be blended with liquid, beyond which the improved
214 performance ceases to prevail.

215 3.4.Wear Mechanism in Extreme Pressure Characteristics

216 The wear behaviour under extreme loading condition is to be studied. Formation of a thin film
217 between two balls was responsible for high seizure load of NO at higher loads as shown in
218 Figure 10 (a). Blok has discussed that there will the surface irregularities which form an
219 interlocking which tends to reduce the surface area of the mating when compared to the
220 apparent area. This reduction in the area causes a very high bearing pressure which tends to
221 form a strain hardening [65]. This is avoided by formation of the thin film which avoids the
222 steel ball getting in contact with each other and prevent them from getting worn out. After
223 certain loading, the thin film fails to form which gets the metal surfaces in contact. This contact
224 region is the high thermal zone leading to high temperature. Syahrullail et al. found that during
225 extreme pressure on vegetable oils the wedge cutting edges will be formed due to high load
226 [66]. In the present study, the wear scar was observed under an optical microscope, both
227 abrasive and adhesive behaviour was noticed.
228 The wear mechanism after blending GNPs with NO is unlike to the condition without GNPs.
229 The thin films are formed even at very high loads which indicates the fulfilment of the role of
230 GNPs in improving the tribological properties. The minuscule GNPs will diffuse between the
231 balls and some GNPs are stopped by the wear scar formed and they settle in the wear scar
232 region over which the balls slide. GNPs being multi-layered experiences a shear force and
233 avoid the metallic contact thereby increasing the seizure load. Thin film formation just before
234 seizure load with 0.5% GNPs-NO and 1.0% GNPs-NO is shown in Figure 10 (b) and (c). The
235 film thickness is shown varied because of exposure of the oil film to a very high load.
236 Apparently, load at the seizure is high and the viscosity is also varied. Xu et al. have proved

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237 that the graphene adheres to the wear scar which acts as a solid lubricant and sustain the high
238 load up to a certain level [67].
239

240
241 FIGURE 10: Illustration of formation of thin film between balls just before the weld: (a) 0.25 wt. % GNPs-
242 neem oil, (b) 0.50 wt. % GNPs-neem oil, (c) 1.0 wt. % GNPs-neem oil .
243 Figure 11. shows the shearing of GNPs when exposed to a very high load and high speed of
244 operation. The amount of the GNPs present is 0.25% and 0.5% GNPs-NO obliged to the
245 explanations put forth by Xu et al. [67]. Abrasive wear occurs because of the presence of more
246 amount of GNPs in a unit volume considered. Hence, removes the material from steel balls and
247 form debris. The material removal is associated with high-temperature generation due to the
248 metallic contact, which in turn causes the seizure by joining the steel balls. Zhang et al.
249 investigated with oleic acid modified graphene at 5 wt. % showed abrasive wear behavior [68].
250 There is one more reason which also has some critical influence on seizure load that is
251 aggregates of GNPs bigger than thin film formed by the liquid can’t diffuse in between the
252 steel balls paving a way to more wear and instant weld [69].

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253
254 FIGURE 11: Illustration of shearing of GNPs at high loads in case of 1.0 wt. % GNPs-neem oil.

255 3.5.Metallurgical Aspects Involved in Welding of Balls

256 It is required to focus the effect of the high load adhesive wear on the metallurgical parameters
257 and metallurgical modifications that occurs in steel balls. In this regards, Ming Feng has
258 discussed that the metallic surface in contact and in relative motion with each other forms
259 grooves and the ridges. Consequently, this formation is followed by strain hardening. It was
260 also mentioned that there will be debris formation or shear that takes place which raises the
261 temperature to such an extent which is sufficient to melt the steel at the contact point and stick
262 it to one of the mating surfaces [70].
263 Similar to the conditions discussed by Syahrullail et al. Figure 12. (a) shows the wedge cutting
264 edges found in case of NO oil [66]. The wedge cutting edge is formed due to the high load and
265 high speed of operation which further leads to high temperature and cause the metal to melt.
266 However, the edges exposed to the very high thermal atmosphere caused a partial seizure which
267 indicates the approaching weld point. At the seizure load, a severe shear took place at the point
268 of contact creating a huge temperature and joining of steels balls takes place this proves the
269 adhesive seizure.
270 It was observed that the balls were exposed to a very high load of order 2.3kN and high
271 operational speed the balls start welding and de-welding which in turn causes the adhesion
272 wear. Adhesion wear further leads to the micro joint of the metal from stationery balls to its
273 counterpart. In this study, above mentioned case can be clearly observed in Figure 12 (b) to
274 (d). This adhesion phenomenon forms a pit on the ball surface while examining. As evidence,
275 Pits were observed in optical microscope image taken from the optical microscope coupled
276 with the Four-ball tribometer. Zulkifli et al. have discussed that the steel balls form a micro
277 joint with each other due to the adhesive wear and this micro joint when ruptures form a pit
278 [71]. In Figure 12, when compared to NO and 0.25 % GNPs-NO, wear pit observed with the
279 NO modified with 0.5% GNPs-NO is lesser Figure 12 (d) because at such a high load the metal
280 will squeeze out to the edges forming the wedge cutting edge rather than adhering on to the
281 rotating ball surface. This phenomenon can be visualised in Figure 12 (a). However, the
282 formation pits seem to be more significant in the NO and 0.25% GNPs-NO.
283 The bulk matter squeezed out from the edges due to the melting of balls. The noteworthy reason
284 is that due to very high load, a temperature gradient was observed in steel balls and this
285 temperature gradient decreases the hardness value, in turn causing metal to melt and squeeze
286 in case of 0.5% GNPs-NO.

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287 FIGURE 12: (a) Shows the formation of thin films just before weld. (b) Pit formation (adhesion wear) in case of
288 NO. (c) Pit formation in case of 0.25% GNPs-NO. (d) Pit formation in case of 0.5% GNPs-NO.

289
290 FIGURE 13: Metal squeeze out due to high load in case of NO+0.5 wt. % GNPs.
291 4. Conclusions
292 The current investigation presented the possible enhancement of the viscosity, wear preventive
293 and extreme pressure characteristics of neem oil via the inclusion of 0.25-1.0% GNPs-NO.
294 GNPs were around <50 nm, flake form and very much scattered, utilizing ultrasonication in

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295 the neem oil as base lubricant. On the basis of results presented in the preceding section, a
296 round of the real discoveries is as per the following:
297  The viscosity of pure neem oil diminished as for temperature and expanded with respect
298 the GNPs loading (0.25-1.0 wt. %) for the temperature range of 300C-550C of the
299 examination.
300  The tribological examination of neem oil with low filler loading of graphene nanoplatelets
301 (GNPs) as additives particularly 1.0% GNPs-NO indicated huge decrease in the friction
302 coefficient and wear scar length. This could be because of the better dissolvability of GNPs
303 in steel ball surfaces; these nanoparticles offer better anti-wear ability.
304  Tribological testing demonstrates that the utilization of GNPs is effective for the decrease
305 of coefficient of friction and wear with expanding loading of GNPs. The utilization of
306 higher loaded GNPs (1.0 wt. %) is more compelling than the utilization of pure neem oil.
307 Likewise, the capacity of nano-lubricant for friction and wear reduction depended not just
308 on the tribological behaviour of the nanoparticles, yet in addition on the dispersion pattern
309 of nanoparticles in the neem oil.
310  The patterns of the varying coefficient of friction demonstrate that friction and wear
311 reducing graphene nanolayer forms amid the tribo-testing.
312  The surface roughness of the steel ball improved with increase in the loading of GNPs.
313 Optical micrographs of the wear spots indicate smooth surface, diminished wear scar length
314 with the nanoparticles adhered on the contact surface during the wear test of the neem oil
315 with GNPs. The distinctive structure of the formed friction surface is clearly seen in the
316 contact zone and over the remainder of ball surface.
317  Incorporation of GNPs into neem oil brought about an increase of the load carrying capacity
318 of the bio-lubricant up to 27.7 percent with 0.5 % GNPs-NO. However, the seizure load
319 was expanded by 2.8 percent with 1.0% GNPs-NO loading. This could be expected to their
320 tribo-sintering onto the surfaces and their spacer impact because of their larger surface area
321 and the formation of thin graphene layer on the ball surface.
322
323 5. Acknowledgements
324 This work was funded by The National Institute of Engineering, Centre for Research &
325 Development (NIE-CRD) and TEQIP-III, NPIU. The authors would like to acknowledge the
326 support of Board of Management, NIE, Principal Dr G Ravi and TEQIP-III Coordinator Dr
327 BN Yuvaraju. Thanks go to the following Centre for Composite Materials Research (CCMR),
328 NIE, technical staff Mr. Byresh and Mr. M. Madhusudhan for the help rendered in conducting
329 experiments.
330
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