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。     

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.     

Total vegetable oil greases

A grease has two major constituents, namely, a lubricant, that performs the function of lubrication; and a gellant, that provides a solid continuous phase, occludes the lubricant, and gives apparent physical structure to the grease. Generally, the gellant is 5–30% and the lubricant 65–90%, additives and fillers making up the rest. In conventional greases, the gellant is a vegetable oil soap, and the lubricant is a liquid oil of petroleum origin or is a synthetic. Such greases have limited biodegradability, because the major constituent, i.e., the lubricant, is normally not biodegradable. In total vegetable oil grease, both the gellant and the lubricant are derived from vegetable oils, giving a grease of potentially high eco‐compatibility. Esters, dibasic acid esters, and alkylated esters of vegetable oil are known to be high‐quality lubricants. These can be used with soap stocks prepared from vegetable oils to give a grease of total vegetable oil origin. The vegetable‐oil based lubricants and soaps are prepared separately and combined in appropriate proportions to give a grease of the required specifications. Alternatively, esterification and saponification can be carried out simultaneously to give a grease of the desired specifications, where an alkali will be the catalyst for esterification, and reactant for saponification. In this paper, the process parameters, and kinetics of these simultaneous reactions are discussed. The results of experimental evaluation of some of these greases are also presented.     

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.     

Tribological characteristics of bisphenol S bis(diphenyl phosphate) as a high‐performance antiwear additive in lubricating greases at elevated temperature

Bisphenol S bis(diphenyl phosphate) (BSDP) was synthesised and characterised, and its tribological behaviours as additives in polyurea grease and lithium complex grease were evaluated for steel/steel contact at 200 °C. The results indicated that BSDP could dramatically reduce the friction and wear of sliding pairs in the base grease of polyurea, and the tribological performances of BSDP in polyurea grease were significantly superior to the normally used molybdenum disulfide‐based additive package. Furthermore, BSDP in polyurea grease has better tribological behaviour than that in lithium complex grease at a constant load of 100 N. X‐ray photoelectron spectroscopy analysis indicated that boundary lubrication films composed of Fe(OH)O, Fe₂O₃, Fe₃O₄ and FePO₄ compounds containing the P–O bonds and nitride compounds were formed on the worn surface, which resulted in excellent friction reduction and antiwear performance. Copyright © 2016 John Wiley & Sons, Ltd.     

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.     

Speed‐ and topography‐dependent boundary friction characteristics of steel

A novel tribometer that undergoes significant changes at ultra‐slow (>5.0 µm s⁻¹) to moderate (<20 cm s⁻¹) sliding speeds was developed in order to study the friction‐speed characteristics of steel lubricated with oil. Three different surface topographies were applied to the specimens, and the friction characteristics with an additive‐free base oil (MO91) and a stearic acid‐formulated oil (StA/MO91) were studied to understand the effects of surface textures on the lubrication performance of an adsorbed molecular layer formed by StA. Friction reduction behaviour of the adsorbed layer observed in the transverse direction was attributed to microscopic hydrodynamic action that maintained the load‐carrying performance of the adsorbed layer. Copyright © 2010 John Wiley & Sons, Ltd.     

Film Forming Behavior of Greases Under Starved and Fully Flooded EHL Conditions

Improving knowledge on the film forming behavior of greases is essential to be able to develop efficient greases. This article examines how operating conditions (e.g., temperature, lubrication condition [fully flooded/starved]) and base oil viscosity influence the film forming properties of greases by comparing the behavior of two lithium-based greases and their respective base oils in rolling point contact. It is found that the onset and degree of starvation is controlled by speed (u) × viscosity (ν)/load (W) factor (uν/W) and temperature and that low uν/W values promote entrainment of thickener into contact. Thus, grease with low base oil viscosity shows significant thickener entrainment in the low speed region compared to the one with high base oil viscosity, which leads to the formation of thickener-rich viscous material during extended running with the low base oil viscosity grease. The results suggest that the shape of the film thickness versus speed curve is viscosity and uν/W range dependent. Furthermore, for the test conditions used in this study, grease-lubricated contacts appear to shift from the initial fully flooded condition to starved condition over a prolonged running of 2 h. The results from this study concur with those reported in the literature that fully flooded oil elastohydrodynamic lubrication (EHL) theory or film thickness cannot be directly applied or taken as a guideline in grease-lubricated contacts.     

几种金属纳米粒子作润滑脂添加剂的试验研究

用Falex四球摩擦磨损试验机考察了镍、钴、铬、钼、铁-钴及铁-镍合金纳米粒子作为添加剂加入润滑脂的摩擦学行为。结果表明：添加纳米粒子的润滑剂均具有较好的减摩抗磨性能和较高的承载能力(PB值)，合金纳米粒子比金属单体纳米粒子的添加效果好，纳米粒子质量分数在3％左右时润滑脂具有较佳的摩擦学性能。     

Starved Grease Lubrication of Rolling Contacts

Many grease lubricated roller bearings operate in the starved elastohydrodynamic (EHL) regime where there is a limited supply of lubricant to the contact (1). Under these conditions the film thickness drops to a fraction of the fully flooded value (2) and, thus, it is difficult to predict lubrication performance, or bearing life, from conventional EHL models. In this regime film thickness depends on the ability of the grease to replenish the track rather than the usual EHL considerations. The conventional view of grease lubrication is that base oil bleeds from the bulk reservoir close to the track, replenishing the inlet and forming a fluid EHL film (3). Resupply, under starved conditions, will thus depend on both operating conditions and grease parameters. The aim of this paper is to evaluate the influence of these parameters on starved lubrication in a rolling contact. Starved film thickness has been measured for a series of greases and the results have been compared to the fully flooded values. These show that the degree of starvation increases with increasing rolling speed, base oil viscosity and thickener content but decreases at higher temperatures. In many cases an increase in absolute film thickness is obtained when moving from high viscosity base oil to a low one, this result is the reverse of normally accepted EHL rules. Taking the fully flooded film thickness as a guide to lubrication performance is therefore not valid as grease film thickness in the starved regime is determined by local replenishment rather than bulk rheological properties.     

Influence of grease rheology on thrust ball bearings friction torque

The friction torque and the operating temperatures in a thrust ball bearing were measured for seven different types of greases, including three biodegradable greases having low toxicity. These friction torque tests were performed using a modified Four-Ball machine.Rheological evaluations of the lubricating greases were made using a rheometer. Bleed oils were extracted from the greases and the dynamic viscosities were measured.In order to compare the performance of the lubricant greases in terms of friction, the grease characteristics were related to experimental results, showing that the interaction between thickener and base oil have strong influences in the bearing friction torque.     

Differences in Mechanisms for Fretting Wear Reduction between Oil and Grease Lubrication

The different mechanisms of fretting wear in oil and grease lubrication and methods to reduce fretting wear were examined by means of thrust ball bearings in this study. Tests of fretting wear under oil lubrication were conducted. It was confirmed that high-viscosity oil can reduce fretting wear at high velocity (i.e., high frequency) through oil film formation. In the case of grease lubrication, the influence of velocity on fretting wear was significantly different for low- and high-viscosity greases. Grease with low-viscosity base oils could reduce fretting wear at high velocity. In contrast, grease with high-viscosity base oils could reduce fretting wear at low velocity. Grease thickeners were found to be effective in forming a layer that could prevent fretting wear. These results highlight the large differences in effective fretting wear reduction mechanisms between oil and grease lubrication.     

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.     

Formation of Low-Friction Particle/Polymer Composite Tribofilms by Tribopolymerization

Inorganic fullerene-like (IF) solid lubricant particles based on MoS₂ or WS₂ have recently gained attention in various tribological applications, for instance incorporated in coatings, porous materials, greases and dispersed in oils. However, their effect in oil can be limited often due to inadequate penetration into the contact zone. Meanwhile, tribopolymerization of monomer additives in oil have proven to be efficient to reduce wear, but without significantly reducing the friction. This investigation combines these two lubrication techniques in order to form particle/polymer composite tribofilms, aimed to give low friction and wear in high-pressure sliding contacts. A cyclic amine, caprolactam, was used as the monomer together with IF as well as normal 2H WS₂ particles. Zn-DTP was used as a reference antiwear additive and poly-alfa-olefin (PAO) was used as the base oil. Reciprocal ball-on-flat sliding test results found that monomer plus particles reduced the friction by 10–50%, depending on sliding speed and type of particles, compared with particles or monomer alone. And the scattering between different tests was also considerably lower. The wear rate was also substantially reduced to a level similar to that of Zn-DTP. The particle/polymer composite tribofilms were generally much larger than the actual contact area and its thickness varied from below a few nanometres in the contact centre to several micrometers in the outer parts. Consequently, the reduced friction is believed to come from two effects: one being a trapping of particles in the contact zone, which reduces the boundary friction level; and the other a shift in lubrication regime towards EHD-lubrication due to reduced contact pressures accompanied with the formation of the composite tribofilm.     

Topography-related effects on the lubrication of nanostructured hard surfaces

This study reports the effect of nanoscaled surface structure of some hard coatings on the (micro-) frictional behaviour of systems under minimum lubrication conditions with modest contact pressures and low sliding speeds (below 1 mm/s). For this purpose, Cr-N coatings with a randomly crater-like topography and with varying dimensions of surface features as well as a smooth Cr-N surface were tested with a microtribometer. The friction on the samples was measured as a function of the viscosity of the applied mineral base oil and the sliding velocity. For all tests, the structured surfaces exhibited lower friction than the smooth surface. Furthermore, it was possible to detect variations in the lubrication-promoting effect of the structures depending on the oil viscosity and the sliding speed. Indications for the existence of an optimum topographic scale for this type of surface structure were found.     

有机无灰减摩剂对流体动压润滑减摩性能影响机制

有机无灰减摩剂能减低流体动压润滑摩擦因数,对提升流体动压润滑性能提供了新思路。采用单油酸甘油酯、油酸、季戊四醇四异硬脂酸酯、司盘80作为有机无灰减摩剂,以质量分数5%与PAO 5基础油进行调和,制备4种不同润滑油样,采用流体动压润滑试验机对比其摩擦学性能。试验结果表明,有机无灰减摩剂在边界润滑和混合润滑中均具有一定减摩效果,在流体动压润滑下减摩效果更明显。其中,含质量分数5%季戊四醇四异硬脂酸酯的油样具有最佳的减摩作用,其在流体动压润滑状态下可使基础油的摩擦因数降低19.6%。分子动力学模拟结果显示,有机无灰减摩剂在摩擦表面产生滑移现象,减少了分子间碳链的相互缠绕,进而降低流体动压润滑下的摩擦因数。     

Analysis of antiscoring and antifriction properties of greases

The paper describes an improved electric circuit of the method for estimating the scoring resistance of greases based on contact resistance measurement. Antiscoring and antifriction properties of greases under conditions of sliding and rolling friction are studied. The critical loads for the greases under testing are determined and the grease having the best antiscoring and antifriction properties is selected.     

The Slow-Speed Wear Behavior of Case-Carburized Gears Lubricated with NLGI 00 Grease under Boundary Lubrication Conditions

NLGI 00 greases are often used to lubricate gears running at low pitch line velocities, such as, for example, in large open gear drives. At low pitch line velocities, sliding wear, which under these operating conditions is referred to as slow speed wear, is often the limiting factor to gear lifetime. A thorough knowledge of the effect of different grease components on the wear behavior is therefore important when selecting a grease to effectively reduce gear wear in a given gear drive. In order to systematically investigate and analyze the influence of different grease components on the slow-speed wear behavior of case-carburized gears, systematic gear tests using the Gear Research Center's (FZG) back-to-back gear test rig were conducted. Primarily, the focus of the experimental investigations is on the influence of the base oil viscosity and type, the additive type, and also the type of soap thickener on the gear wear behavior at low pitch line velocities. To experimentally determine the influence of these different grease components on the wear behavior of case-carburized gears, a modified, more stringent wear test, based on the standard DGMK slow-speed wear test for gear oils, was developed. Different NLGI 00 greases with base oil viscosities between ν₄₀ = 70 and 1,200 mm²/s were investigated.

Base oil type and base oil viscosity were shown to have only a minor effect on the wear behavior under boundary lubrication conditions. On the other hand, the thickener type and especially the additive type play an important role in determining the wear behavior.     

Self-diffusion of oil in lubricating greases by NMR

Self-diffusion of base oil in six model lubricating greases and in the base oils themselves was measured using pulsed-field gradient nucleic magnetic resonance (NMR) at 23, 40, 70, and 90°C. Three of the greases were based on naphthenic mineral oils, and three were based on synthetic polyalphaolefin oils. Soaps of 12-hydroxy stearic acid were used as thickener agents in all six greases. The purpose of the investigation using NMR was to see if structure varies with temperature, and if NMR is a viable method for structure determination. The ratio between the diffusion coefficient of the base oil in the grease and the neat base oil in itself was evaluated as a function of temperature. This ratio was taken as a direct indicator of the obstruction effect that the thickener has on the oil. The thickener showed a stronger obstruction effect on the base oil in the synthetic grease than in the mineral-based grease. This was related to the soap content, which, for these greases, is roughly twice as high in the synthetic greases as in the mineral ones. The obstruction effect was constant in the temperature range 40–90°C for mineral- as well as synthetic-based greases. NMR was judged to be a promising method for investigating how the gellant affects the diffusion coefficient of oil in a lubricating grease.     

Film thickness in a ball-on-disc contact lubricated with greases,bleed oils and base oils

Three different lubricating greases and their bleed and base oils were compared in terms of film thickness in a ball-on-disc test rig through optical interferometry. The theoretical values calculated according to Hamrock's equation are in close agreement with the base oil film thickness measurements, which validates the selected experimental methodology.The grease and bleed oil film thickness under fully flooded lubrication conditions presented quite similar behaviour and levels. Therefore, the grease film thickness under full film conditions might be predicted using their bleed oil properties, namely the viscosity and pressure-viscosity coefficient. The base and bleed oil lubricant parameter LP are proportional to the measured film thickness.A relationship between grease and the corresponding bleed oil film thickness was evidenced.