co») United States c2) Patent Application Publication (o) Pub. No.: US 2018/0291305 Al Kumar Tompala et al. (4) Pub. Dat US 20180291305A1 Oct. 11, 2018 os) om om (0) Oct. 6, 2015 NANO SUSPENSION LUBRICANTS Applicant: Hindustan Petroleum Corporation Limited, Mumbai (IN) lveators: Annaji Rajiv Kumar Tompala, Benglura (IN); Srinivas Vadapall Visakhapatnam (IN); Amitabh Kumar Jain, Navi Mumbai (IN); Venkata Chalapathi Rao Peddy, Benglura (IN): Venkateswarlu Choudary Nettem, Benglura (IN); Sri Ganesh Gandham, Visakhapatnam (IN) Appl. Nos 15/766.509 PCT Filed: Jun, 30, 2016 PCT No: PCTIIN2016/050208, $371 XD, (2) Date: "Apr. 6, 2018 Forsign Application Priority Data a 3793:MUM/2015 on) on Publication Classification Int. Cl. c1OM 17106 2006.01), cum 1700 (2006.01) cioM 01m (2006.01) C10 171/06 (2013.01); C1ON 227000 (2013.01); Cross 101/02 (2013.01): Clo 2201/05 (2013.01); C1OM 2201/066 (2013.01) ‘C1OM 2203/1006 (2013.01); C1OM 2207/126 (2013.61); CLOM 3207/289 (2013.01); C1OM 2215704 (2013.01); CLON 2220/082 (2013.01) CION 2220084 (2013.01); CLON 2230/06 (2013.01); CION 2230110 2013.01); CION 230/12 (2013.01); C1OM 17700 (3013.01) ABSTRACT A meshed! for preparing « nano suspension lubricant com: prises providing substantially spherical nano particles of size ranging from about less thin SO nanometers to about 100 ‘nanometers. The method further comprises mixing the nano particles and a surfactant in about 1:1 ratio in @solveat to orm a mixture. The solvent is evaporated from the mixture to obtain surface modified nano particles, The surface mod fied nano particles include the nano particles coated withthe surfactant: The method eomprises mixing the surface mod. fied nano particles with a Ibrcating fui to form the nano suspension lubricant, where the lubricating fiid comprises bout 90% t0 99% base ol and about 1% to 10% additives re PROVIDING SUBSTANTIALLY SPHERICAL NANO PARTICLES DISSOLVING THE NANO PARTICLES AND A SURFACTANT IN ABOUT 1:1 RATIO IN A SOLVENT EVAPORATING THE SOLVENT IN ROOM TEMPERATURE TO (OBTAIN SURFACE MODIFIED NANO PARTICLES THING THE SURFACE HODIFIED NANO PARTICLES WITHA LUBRICATING FLUID, WHERE THE LUBRICATING FLUID CCONPRISES OF ABOUT 90% TO 29% BASE OIL AND [ABOUT 1% TO 10% ADDITIVESPatent Application Publication Oct. 11, 2018 Sheet 1 of 26 US 2018/0291305 Al r” PROVIDING SUBSTANTIALLY SPHERICAL NANO PARTICLES. 102 104: DISSOLVING THE NANO PARTICLES AND A SURFACTANT IN ABOUT 1:1 RATIO IN A SOLVENT 106 EVAPORATING THE SOLVENT IN ROOM TEMPERATURE TO. OBTAIN SURFACE MODIFIED NANO PARTICLES 108 MIXING THE SURFACE MODIFIED NANO PARTICLES WITH A’ LUBRICATING FLUID, WHERE THE LUBRICATING FLUID COMPRISES OF ABOUT 90% TO 99% BASE OIL AND ABOUT 1% TO 10% ADDITIVES Fig. 1Patent Application Publication Oct. 11, 2018 Sheet 2 of 26 US 2018/0291305 Al arbitrary unit (2.u ) ‘on 1090 B90 200 Diffraction Angle (22) Fig. 2US 2018/0291305 Al Oct. 11,2018 Sheet 3 of 26 Patent Application Publication (p)¢ “614 (q)e “614 ove 4 (9)¢ “B14 SSPARIOURN ZAVPOPOL! SPURSOUN ZAWPOYOL SSSEOPAATPIA SITERSOPRAL HIN ARSE SADPIRY = | i * om ~ OTFUS 2018/0291305 Al Oct. 11,2018 Sheet 4 of 26 Patent Application Publication (ue “614 Da TO RHO URLS DORA DS SmUAANOMR A sD «woos —4 We ‘64 spuslascavpun ——Spussianicsiema pee) 88 SEPERTONNERSIND SoMETOMAKEIIP-D SpuanrobaE9s150 00s 4Patent Application Pt ublication Oct. 11, 2018 Sheet 5 of 26 US 2018/0291305 Al on $1 = one = 006 = oot 2 002 H 0 Joon crowd ana = 3 | Deelagre | Oeelerire | Deslagre Desdengneciho | inO0b%esuface | AhO1Ssuface | N02 surface Sénanopartides | madfedNbS2 | medfedMts2 | reed Ms? . | | rnopaties _ | friction results i foie 160 | uo | _ ml 2 0} 3 | 2 a0 | Pol “ 40; 2») | oF ~~] bieselengine | Dieselengine | Dieselengine | | Diesel engine oilO | oil40.05% surface | oilt0.1%surface | ollt0.2%surface | | sémonopartides | modified Mes? | medfied MoS | modified MoS? | | ne parties “rane paticles | setae lond i | 10 100Patent Application Publication Oct. 11, 2018 Sheet 6 of 26 US 2018/0291305 Al oa 008 0.06 Coetfent of friction 008 oo Seizure lad, kef ame il vtuoltngiee | Petoltngine | Petrol fngine Petrol Engine | Pevoltngine | gusoastesurtace | ol INSurice | ob-01% Sure won Nano |“ potiied MoS? | modlied MoS? | modified Mos? | articles | _Nano Particles | Petrol engine 60.05% Surface | oils.1% Surface Petra Engine cilvoa%surtece | cH0% Nano | ated most | modited most | modhedwost | oracles | 130 JPatent Application Publication Oct. 11, 2018 Sheet 7 of 26 US 2018/0291305 (ae oa 008 006 008 002 ah , a a Lay z 3 Tears] Gear a |e AE cearoisae | sowsorons% | aowoowar% | sowsa}02% sonst} rao | Surscemodied | surface modiied | sucace modes pater | MoS2rano. | MaSanano | MaS2rano, | Lees | ares tut 180 | 160 | 10 | 3 120 | Zw t #9 i @ 40 » ° 1 7 1 Gear ol(SAE | Gear ol SAE] Gearol(sat soveoroos% | sowsoro1x | sowwonor® | ‘Surface modified | Surface modified | Surface modified = MoS2nano | —-MoS2nano. |= MoS2nano. antes partes | fw ciareload | 16060 |Patent Application Publication Oct. 11, 2018 Sheet 8 of 26 US 2018/0291305 Al on o1 | o08 Gearait | Cocttident of trition a Gearoil'€P | (EPLMOWOOS% | fEPIAOWO.A% | (ERLAOWO.2% | asojorinano | modified | Surface modfed | Surface modified parties | MoS2nano.—| = MaS2nano— | MoS2nano | | _patides | parides | __ parties L [oon ors P00. 160 0 e 3 te $6 i “ 40 0 oF r — — — Geral | Gearol | «Gara Gearoiter | (eridopansse | (ertaoywo% | (ePteow0.2% s40}e0%nano | Surface moaiied Surface modified | Surface modified par Mosznane | MaS2nano— | MaS2nano ortides partiesPatent Application Publication Oct. 11, 2018 Sheet 9 of 26 US 2018/0291305 Al ame boos 2 xo} | °F r I90, 2190 oi ASINDSWO 56 37 sa ASIN D293 12012000 >iUS 2018/0291305 Al Oct. 11, 2018 7 TABLE 1.2-continaed ont hae un unas Maa Bate bit + Bis ot « sk rest aa osteo 0% NO, PROPERTIES METHOD —_luwicur__" cper csr High Tempo High Seach AST DAMS 79 wr sa 1 rte AST Ds is w 1s Gomeranpeorosona ap ASIMDISN IA ann 16 ConnionCabee ene ASTD I 2. 278 10097) The test results tabulated in table 1.2 indicate chat ‘TABLE 14 thers mo sianitcant change inthe physio-chenal prop erties of the nano suspension Iubricnt tit may render the nano suspension irient unstable for use in the suomo- tive ewironment [0098] The tribological propre, such as tion ri tance, wear resistance, ef, ofthe copper base nano su pension lubricant is also tested evaluat improvement in Iubicting. properties of the nano suspension fbrcant Table 13 states the same [0099] detiled Tribogical analysis and testing is being done as per ASTM G59 standard on pin on dsc tibometer Pro to conducting the es, the dics ae ground ite grinding machine and ensured tobe smooth nifty ‘The surface roughness is checked for all dises under testing dense that thy are inthe same ange (02-04 um a) ‘This is done to ensure that ll th tests are conducted under the same contons to achieve ufo [0100] The test conlitions are Fisted below: [O101] Load: §, 10,15 & 20 kat {0102] Spe of rotation 300, 600, 1200 RPM {0103} Pin & Dise materials: Cason TABLE 13 ‘Vatsion in cote of ficion ofthe cope bas nan sues Ici a ring of resting po ona se tir i is Change fom base Acres Cofino ston uit Seat Be ch ROM rest 086 ls U2 Ost IMO. Go ARK DOM? ONO DOI 07) oe Mae jon eans nas osze os1s go gm 2222 1200087 O46 0865 00388 SHAT DNS 25.49 i may be noted ftom the above table thatthe copper based nano suspension lubricant exhibits improved friction resi tance. [0104] Teibotogical Testing with ASTM 4 Ball Wear Tes- ter [0105] ‘The wear preventive and ant-ition properties of the lubricants mixed with nano particles are being evaluated using ASTM 4 ball wear tester. As per ASTM D 4172, the ‘war preventive properties ofthe nano suspension lubricant ‘ean be characterized fromthe test results tabulated below. via ‘east ine mate Bee hivoa Bae lat + 015% Cu aoe pres Base lat #14 Cu mane piles St as 2 [0106] 1 may be noted from the wear sear diameter has substantially reduced with inerease inthe weight % of the surface modified copper nano particles dispersed in the lubricating Nuid. This indicates improvement in wear pre- ventive properties of the copper based nano suspension lubricant, [0107] X-Ray Diffraction (XRD) Analysis [0108] Metllographic studies are conducted to assess the reduction in wear die to use ofthe nano suspension ubricant secording to an example implementation. After conducting wear tess, the balls of wear test are subjected to XRD analysis for analysis ofthe possible deposition ofthe copper ‘nano patiles on surfaces of the worn balls. FIG. 2 graphi- cally illustrates the XRD analysis test results for the copper, based nano suspension lubricant according to an example implementation. Te graph 200 shown in FIG. 2 depicts the ‘amount of deposition ofthe copper nano putcles present in the nano suspeasion lubricant onto the worn out surfaces of the motalic balls. In x-axis a diffraction angle ofthe X-ray dilaetion is ploted and inthe y-axis the amount of depo- sition ofthe copper nano particles on the surface ofthe worn ‘our metalic balls is depiced. The diffraction angle is measured in degrees and the amount of deposition is expressed in an arbitrary unit of number of eycles of measurement in the XRD, From the FIG. 2 it may be noted that along with iron (Fe), Nickel (Ni), Chromium (Ct) and oxygen (O) copper (Cu) can also be seen at peaks of the raph 200, This suggests deposition of the copper nano particles on the surface of the worn out balls and fom a protective coating thereby offering resistance to wear [0109] Friction Test as Per ASTM D 5183 Stand [0110] ‘The fiction test hes been conducted to determine the eoellcient of friction ofthe copper based nano suspen sian lubricant under the following peesribed test conditions using the ASTM 4 Ball wear tester, [0111] The test is conducted under the following test conditions [0112] Temperature 7522" C. [0113] Speed 600 RPM.