Study of the Conductivity and Tribological Performance of Ionic Liquid and Lithium Greases

Ionic liquid (IL) lubricating greases were prepared using 1-hexyl-3-methylimidazolium tetrafluoroborate and 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide as base oil and polytetrafluoroethylene (PTFE) as thickener, respectively. Three kinds of lithium greases were also prepared using lithium ILs ([Li(PAG)]X) as base oil and PTFE as thickener. 1-Ethyl-3-methyl imidazolium hexafluorophosphate as an additive was added to the PAG grease, which was prepared using polyalkylene glycol monobutyl ether (PAG) as base oil and PTFE as thickener. The conductivities and tribological properties of the prepared lubricating greases were investigated in detail. Scanning electron microscopy and X-ray photoelectron spectroscopy were employed to explore the friction and wear mechanism. The results showed that the IL and lithium lubricating greases have conductivities and excellent tribological properties. Especially, IL greases have the highest conductivity. The excellent tribological properties are attributed to the formation of boundary films consisting of both tribo-chemical reaction films and physical absorption films, while high conductivities are attributed to the intrinsic electric fields of the ILs.     

蓖麻油基含氧化石墨烯润滑脂的制备及其性能研究

以蓖麻油为基础油,以一水氢氧化锂、12-羟基硬脂酸和癸二酸为稠化剂原料,氧化石墨烯(GO)为添加剂,制备3种含GO不同质量分数的混合锂基脂,分别利用锥入度试验器、钢网分油测试仪、滴点试验器、流变仪、热重分析仪、摩擦试验机和三维形貌仪考察其理化性能和润滑性能,探讨GO对蓖麻油基润滑脂的作用机制。结果表明:含GO混合锂基脂的黏度随剪切率和温度的增加均呈非线性减小的变化趋势,但随着剪切速率和温度的升高,GO对蓖麻油基润滑脂的黏度与剪切速率关系和黏温特性影响越来越小;微量的GO能够提高混合脂的热稳定性能;混合锂基脂的平均摩擦因数随GO质量分数的增加呈先减小后增大的变化趋势,适量的GO有助于提高蓖麻油基润滑脂的减摩抗磨性能,这是因为摩擦过程中GO以片层形式进入摩擦副的接触区,能够有效地降低摩擦副表面的直接接触概率,且GO具有自润滑性能,在摩擦副界面上发挥较为有效的润滑作用。     

Alkyl Imidazolium Ionic Liquids as Friction Reduction and Anti-Wear Additive in Polyurea Grease for Steel/Steel Contacts

Five room temperature ionic liquids (ILs), 1-butyl-3-methylimidazolium hexafluorophosphate (L-P104), 1-hexyl-3-methylimidazolium hexafluorophosphate (L-P106), 1-octyl-3-methylimidazolium hexafluorophosphate (L-P108), 1-decyl-3-methylimidazolium hexafluorophosphate (L-P110), and 1-hexyl-3-methylimidazolium tetrafluoroborate (LB106) were studied as 1 wt% additives of polyurea grease for steel/steel contacts. Their tribological behaviors as additives of polyurea grease for steel/steel contacts were evaluated on an Optimol SRV-IV oscillating reciprocating friction and wear tester and an MRS-1J (G) four-ball tester at room and high temperatures. The friction test results showed that the ILs, as 1 wt% additives in polyurea grease for steel/steel contacts, had better friction reduction and anti-wear properties at high temperature than at room temperature, and ILs can significantly improve the friction reduction and anti-wear properties of polyurea grease compared with base grease containing 1 wt% of zinc dialkyldithiophosphate (T204). The excellent tribological properties are attributed to the formation of a surface protective film composed of FeF₂, nitrides, and compound containing the P–O bonding on the lubricated metal surface by a tribochemical reaction. The ordered adsorbed films and good miscibility of ILs with the base grease also contributed to the excellent tribological properties. Wear mechanisms and worn steel surfaces were studied by a PHI-5702 multifunctional X-ray photoelectron spectrometer and a JSM-5600LV scanning electron microscope.     

A study on tribological behaviours of ZDDP in polymer thickened lubricating greases

Zinc Dialkyl Dithiophosphate (ZDDP) is a well‐known multifunctional additive for soap based lubricating greases. Polymers are being studied for their performance as lubricating grease thickeners and rheology modifiers. In this work the tribological study of ZDDP was carried out in polypropylene (PP), maleated polypropylene (mPP) and linear low density polyethylene (PE) thickened lubricating greases. Performance of lithium grease was taken as a reference. The tribological properties were evaluated using a four ball tester for EP properties and Optimol SRV‐III machine for coefficient of friction. The mechanism of action of ZDDP in polymer greases was established through analysis of the worn surface of steel balls with scanning electron microscope (SEM) and energy dispersive x‐ray spectroscopy (EDAX). The results show that the performance of ZDDP depends on the thickener system. The antiwear and EP property exhibited by ZDDP varies from polymer to polymer. Poor performance was observed with PP type thickener whereas performance in PE and lithium grease was comparable. Copyright © 2015 John Wiley & Sons, Ltd.     

Rheological and Tribological Characterization of a New Acylated Chitosan–Based Biodegradable Lubricating Grease: A Comparative Study with Traditional Lithium and Calcium Greases

This work compares the thermal, rheological, and tribological properties of a new gel-like biodegradable formulation, prepared using an acylated chitosan thickener and castor oil, with properties exhibited by two conventional greases thickened with lithium and calcium soaps, respectively, taken as benchmarks. Thermogravimetric (TGA), rheological (small-amplitude oscillatory shear [SAOS], rheodestruction, and viscous flow) and tribological (friction and wear analysis) tests, as well as roll-stability measurements were carried out to characterize the three grease samples. In addition, infrared spectroscopy and differential scanning calorimetry (DSC) were used to chemically characterize the acylated chitosan thickener agent. From a thermogravimetric point of view, the new formulation displayed better thermal resistance than the calcium and lithium lubricating greases. The evolution of the linear viscoelasticity functions with frequency and viscosity values in the shear rate and temperature ranges studied were similar to those obtained with the commercial lubricating greases. However, the linear viscoelasticity functions of the biodegradable formulation were slightly more affected by temperature. The mechanical stability behavior and recovery of the rheological functions found in the biodegradable formulation were also better than that exhibited by the calcium-based grease. However, the friction coefficient measured at low rotational speed is slightly higher than that obtained with the benchmarks, with similar or lower values obtained at a high rotational speed. Resulting wear marks obtained after the frictional tests using the acylated chitosan–based grease were larger than those obtained with the commercial greases.     

Tribological Behavior of Amorphous and Crystalline Overbased Calcium Sulfonate as Additives in Lithium Complex Grease

The aim of this study was to examine the tribological behavior of amorphous overbased calcium sulfonate (AOBCS) and crystalline overbased calcium sulfonate (COBCS, transformed from the AOBCS) as additives in lithium complex grease. The transformation product of the calcium carbonate polymorph from AOBCS was calcite, as determined by Fourier transform infrared spectroscopy. Tribological properties were evaluated by an oscillating reciprocating friction and wear tester and a four-ball tester. The results showed that the addition of COBCS can dramatically improve both the antiwear performance and the friction-reducing and load-carrying properties of the base grease. However, improvement of the tribological properties of the base grease by AOBCS was highly dependent on the concentrations added and the loads applied. The tribological properties of the base grease were improved more by the addition of COBCS than by the addition of AOBCS. X-ray photoelectron energy spectrometry and thermogravimetric analysis revealed that both AOBCS and COBCS underwent complicated tribochemical reactions in the base grease and that chemically reactive films consisting of CaCO₃, CaO, iron oxide and organic compounds were formed on the worn surfaces. Taken together with the results of the tribo-tests, we suggest that transformation of the calcium carbonate polymorphs was the main factor in improving the tribological properties of lithium complex grease. The transformation of calcium carbonate polymorphs can broaden the application of AOBCS as an extreme pressure/antiwear additive in greases under boundary lubrication conditions.     

含纳米CuO锂基润滑脂摩擦学性能研究

为改善锂基润滑脂摩擦学性能,制备不同添加量纳米CuO改性的锂基润滑脂。采用3H-2000PS2比表面及微孔分析仪对纳米CuO粒子进行表征,采用四球摩擦磨损试验机分析纳米CuO添加量对锂基润滑脂摩擦学性能的影响,采用扫描电镜(SEM)和三维形貌分析仪分析试验后钢球磨痕形貌。结果表明:纳米CuO质量分数为0.60%时锂基润滑脂具有最佳的抗磨减摩效果,摩擦因数和磨斑直径较基础脂分别降低24%和12%;一定添加量下,纳米CuO对磨损表面具有修复作用,含质量分数0.60%纳米氧化铜的润滑脂润滑时,磨损表面具有较低的表面粗糙度和较少的犁沟,表现出最佳的抗磨性能。     

An assessment of beeswax as a thickener for environmentally friendly lubricating grease production

Environmentally friendly lubricants are preferred in many applications where groundwater or soil pollution is possible. The main purpose of the current study was to evaluate the possibility of beeswax use as a thickener for lubricating greases. European beeswax was used as a thickening material for the preparation of lubricating greases. Rapeseed oil and two mineral oils were used as base oils. The consistency, dropping point temperature, and tribological properties of the prepared lubricating greases were investigated and compared with conventional soap‐thickened greases. The prepared greases exhibited good tribological properties, especially the rapeseed‐oil‐based grease. However, tribological properties of conventional lubricating grease were superior to prepared ones. The weakness of the prepared lubricating greases is their narrow working temperature range. However, the beeswax together with rapeseed oil has great potential in the production of environmentally friendly, completely renewable lubricating greases. Copyright © 2014 John Wiley & Sons, Ltd.     

Oil‐soluble lithium salts as novel lubricant additives towards improving conductivity and tribological performance of bentone grease

The tribological and conductive properties of three kinds of lithium salts (LiBF₄, LiPF₆ and LiNTf₂) as lubricating additives in bentone grease were investigated in detail. As compared with the bentone‐based grease, the lithium salts as its additives not only provide excellent tribological properties but also greatly improve the load‐carrying capacity and electrical conductivity. These benefits are strongly dependent on the formation of a versatile boundary lubricating film and ion diffusion of lithium salts through an external electric field effect. Copyright © 2014 John Wiley & Sons, Ltd.     

Conductive Lubricating Grease Synthesized Using the Ionic Liquid

Two kinds of new conductive lubricating greases were synthesized using 1-octyl-3-methylimidazolium hexafluorophosphate and 1-octyl-3-methylimidazolium tetrafluoroborate as base oil and the polytetrafluoroethylene as thickener. The conductivities of the new conductive lubricating greases are higher than the traditional conductive lubricating greases which contains conductive stuffing. In addition, the physical and tribological properties of the new lubricating greases were investigated in detail. The results show that the new lubricating grease show better friction reducing and anti-wear properties than the lubricating grease based on PAO10 at room temperature and 150 °C. The worn surfaces were observed and analyzed by scanning electron microscope and X-ray photoelectron spectroscope. Also, the possible friction mechanisms for the new lubricating greases are proposed.     

基础油对锂基脂安定性的影响

为研究基础油对锂基脂安定性能的影响。在相同酸碱比例、皂份和相同工艺等条件下,采用12-羟基硬脂酸体系稠化相同黏度不同组分的基础油,制备系列通用锂基润滑脂,分析基础油黏度指数、苯胺点和饱和烃含量对锂基润滑脂安定性能的影响。结果表明:随基础油黏度指数、苯胺点和饱和烃含量的升高,锂基脂工作锥入度、抗水喷雾和压力分油增大,而十万次剪切差值和蒸发量减小;基础油黏度指数、苯胺点和饱和烃含量三者与锂基脂安定性能呈现正相关性,与锂皂的溶解性呈现负相关性。     

Tribological properties and insulation effect of nanometer TiO2 and nanometer SiO2 as additives in grease

New greases were synthesized using oleophilic nanometer-TiO₂ and nanometer-SiO₂ as additives. When the additives in naphthenic oil is 0.1 wt%, the alternating current (AC) breakdown strength is enhanced by 10.4% and 8.2% at power frequency, respectively. Also the grease volume resistivities are improved by 23% and 30% compared with base grease, which use naphthenic oil as base oil. The greases tribological behaviors were explored. Scanning electron microscope linked with energy dispersive X-ray spectroscope was utilized in order to analyze these scratches. The good tribological characteristics of nanometer-TiO₂ greases and the good friction-reducing characteristic of nanometer-SiO₂ greases are ascribed to the nanoparticles mechanical effect, and are also ascribed to the protect film generated by Ti and Si deposited or metallic oxide.     

The Preparation and Tribological Investigation of Ni–P Amorphous Alloy Nanoparticles

Amorphous Ni–P alloy nanoparticles were synthesized by chemical reduction of nickel acetate in water reacted with sodium hypophosphite under stirring. The nanoparticles were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). Results of XRD and TEM showed that nanoparticles have an average diameter 100 nm. And XPS analysis indicated that part of the surface of Ni–P amorphous alloy nanoparticles was oxidized. The tribological properties of the prepared Ni–P nanoparticles as an additive in lithium grease were evaluated with a four-ball friction and wear tester. The worn surfaces of the lubricated GCr15 steel were analyzed by means of XPS and scanning electron microscopy (SEM). The lubricating mechanisms were discussed on the basis of XPS and SEM analyses of the worn steel surfaces. The results show that these nanoparticles as a grease additive can effectively enhance the friction-reduction and antiwear ability of lithium grease. Tribochemical reactions were involved for steel–steel frictional pair lubricated with the lithium grease containing amorphous Ni–P alloy nanoparticles, with the formation of a boundary lubricating and protecting film composed of additives of lithium grease and tribochemical reaction products (iron phosphate, iron oxides, nickel oxide, nickel, etc.) of the lubricants. This contributes to improve the tribological properties of the lithium grease.     

The effect of space irradiation on the lubricating performance of perfluoropolyether greases in simulated space environment

In this paper, 2 kinds of commercial perfluoropolyether (PFPE) greases were coated on the polyimide (PI) blocks, which were placed within simulated space environment including atomic oxygen (AO), proton (Pr), ultraviolet (UV), and electron (El) irradiations, and then the tribological performance has been investigated with a ball‐on‐disc tribometer. Results indicated that the MoS₂‐grease showed better lubrication performance than the PTFE‐grease. The changes in infrared spectroscopy induced by Pr and El irradiations were more obvious than that by AO and UV irradiations. Results of energy dispersive X‐ray spectroscopy indicated that Pr and El irradiations caused carbonation of greases, and AO and UV irradiations induced oxidation of greases. Referred to the tribological properties of PI coated with PFPE oil, PI coated with PFPE greases showed minor changes in friction coefficient and wear rate, and the MoS₂ additives could significantly improve the lubrication properties of PFPE greases in simulated space environment.     

钢丝绳脂组成对抗水性能的影响

应用润滑脂抗水喷雾性测定方法,研究基础油黏度、主稠化剂及辅助稠化剂、黏附剂添加量对钢丝绳脂抗水性能的影响。结果表明:随着基础油黏度的增加,钢丝绳脂的抗水性能有明显改善,尤其是黏度为25~56 mm2/s时改善效果最显著;聚丙烯类主稠化剂在改善钢丝绳脂的抗水性能方面优于聚乙烯类;随着辅助稠化剂微晶蜡添加量的增加,钢丝绳脂抗水性能提高,但微晶蜡质量分数大于4%抗水性能改善效果趋于平缓;随着黏附剂聚异丁烯(PIB)、烯烃共聚物(OCP)添加量的增加,钢丝绳脂抗水性能提高,但黏附剂质量分数大于5%时会导致抗水性能变差;聚异丁烯(PIB)对钢丝绳脂抗水性能的改善优于烯烃共聚物(OCP)。     

Impact of Water on the Rheology of Lubricating Greases

The operational life of bearings is often determined by the performance of the lubricating grease. The consistency of the grease prevents it from leaking out of the bearing and provides good sealing properties. The possible ingress of water into the bearing will have a considerable impact not only on this consistency but also on the lubricating ability of the grease. There are numerous applications where water ingress may occur, such as in the steel, food, pulp, and paper industries. Some greases are less sensitive to water than others. No specific guidelines are available to select the proper grease for bearings subjected to water ingress. The goal of the article is to contribute to the development of such guidelines for greases subjected to water ingress by studying the impact of water on grease rheology. Fully formulated, commercially available greases with the most common thickeners and base oils are used as model greases. It will be shown that water strongly influences rheological properties such as zero-shear viscosity, yield stress, and storage modulus. Calcium sulfonate greases were found to become stiffer after absorbing a considerable amount of water, leading to an increase in zero-shear viscosity and yield stress. However, lithium, lithium complex, and polyurea greases were found to soften, with appreciable changes in measured rheological properties.     

Tribological Performance of Lubricating Greases Based on Calcium Carbonate Polymorphs Under the Boundary Lubrication Condition

In this article, we synthesized the calcium sulphonate grease (CSG) based on the calcite using the bright stock (150BS) as the base oil. In order to investigate the tribological performance of lubricating grease containing different calcium carbonate polymorphs under boundary lubrication condition, a calcium sulphonate complex grease (CSCG) based on the vaterite was used as a reference. An oscillating reciprocating friction and wear tester set at a series of applied loads and frequencies was adopted to evaluate the tribological performance under boundary condition. Results showed that the lubricating grease that was composed of crystalline calcite as the partial thickener had excellent friction-reducing and antiwear (AW) properties, regardless of the applied loads and frequencies. The vaterite in CSCG easily experienced a polymorph transformation into calcite or aragonite characterized by Raman spectroscopy. This polymorph transformation was attributed to the highly local friction temperature and activated hydrogen from water or acids oxidated in the rubbing process at high load or frequency. The physical polymorph transformation corresponded to the fluctuations of the friction coefficients, then contributed to the severe wear. XPS analysis indicated that two calcium sulphonate lubricating greases occurred a tribochemical reaction and boundary tribofilms consisted of CaCO₃, CaO, iron oxide and FeSO₄ were formed on the rubbing surfaces. The tribofilm formed by the introduction of the CSG that mainly depended upon the thickeners of calcite structure contributed to an excellent AW protection. The possible boundary friction mechanism for greases based on various calcium carbonate polymorphs was also proposed. Effect of calcium carbonate polymorphs on the tribological performance was discussed.     

导电聚苯胺在润滑脂中的导电能力及减摩抗磨性能的研究

采用导电高分子材料—聚苯胺粉末作为润滑脂导电添加剂,合成新型电力复合脂。分别对制备的电力复合脂的体积电阻率以及接触电阻（铜片）进行测试,并采用往复摩擦磨损试验机对其室温下在钢-铜,钢-钢摩擦副的摩擦学性能进行研究。利用扫描电子显微镜（SEM）观察金属表面并利用能谱分析仪（EDS）对表面元素成分进行分析。结果表明,聚苯胺粉末能够将基础脂的体积电阻率降低2个数量级;当添加量为2%时,在钢-铜、钢-钢摩擦副上均可获得最好的减摩效果;当添加量为5%时,也可在多数情况下获得好的抗磨效果。EDS分析结果表明,在润滑脂中添加聚苯胺粉末能在金属表面生成含氮化学反应膜,同时聚苯胺可以抑制摩擦过程中氧与金属的反应。     

Tribological Performance and Mechanism of Phosphate Ionic Liquids as Additives in Three Base Oils for Steel-on-aluminum Contact

Butylammonium dibutylphosphate and tetrabutylammonium dibutylphosphate ionic liquids (ILs) were evaluated as antiwear additives for steel-on-aluminum contact in three different base oils, a polyalphaolefin, an ester oil and an IL 1-methy-3-hexylimidazolium hexafluorophosphate, respectively, with similar viscosity and different polarities. The friction experiments were carried out on an Optimal SRV-IV oscillating reciprocating friction and wear tester at room temperature. Results indicate phosphate ILs can effectively improve the tribological properties of the base oil, especially the antiwear property, as additives for steel/aluminum contacts. For the base oils PAO10 and PAO40 with different viscosities, the higher viscosity of PAO40 can be beneficial to reducing the friction coefficient. The worn surface morphologies and chemical compositions of wear scars were analyzed by a JSM-5600LV scanning electron microscope and PHI-5702 multifunctional X-ray photoelectron spectrometer (XPS). The XPS analysis results illustrate that the phosphate IL additives in the base oils with different polarities exhibit the same tribological mechanism. A synergy exists between the adsorbed layers and boundary-lubricating films generated from the tribochemical reaction of IL and the substrate surface, which may reduce the friction coefficient and wear volume of the friction pairs.     

Deuterated grease thickener

The ‘Deuterium Isotope Effect’ was investigated as a means of further increasing the oxidation resistance of soap-thickened greases utilized in miniature bearing applications. Using lithium stearate as a model compound, the bearing performance life and induction period for oxidation were determined on four different greases prepared from non-deuterated and deuterated base oil and thickener. The expected increase in oxidation resistance and bearing performance life was observed for the deuterated base fluid; however, the use of a deuterated thickener did not provide any significant improvement. Details concerning the preparation of thickener and grease formulations and their properties are presented.