Synthetic polyurea extreme‐pressure greases

This paper describes the preparation of synthetic polyurea greases and evaluates their performance. The polyurea greases were prepared in situ by reacting diisocyanate with monoamines and ethylene diamine in the presence of a synthetic base oil (polyalphaolefin). Two different extreme‐pressure (EP) additives blended with the prepared polyurea greases were evaluated for their EP activity in four‐ball and Timken tests. The additivated greases gave higher loads, and higher values of weld load in the four‐ball test as compared to the polyurea grease without additive. The blended greases were also found to pass rust, corrosion, oxidative stability, and shear stability tests. The topography of the wear‐scar surfaces was investigated using scanning electron microscopy.     

Technical note: Extreme‐pressure activity assessment of certain nitrogen and sulphur compounds in lithium‐based grease

In this paper we report on the preparation and extreme‐pressure (EP) activity assessment of certain substituted 1‐amino‐3‐aryl‐2,3‐dihydro‐2‐thioxo‐4,6‐(1H,5H)‐pyrimidinediones as additives in a lithium‐based grease. These additives significantly decreased the wear and friction and possessed the ability to increase load‐carrying capacities and weld loads. Two greases were prepared with the above additives, and both greases exhibited lower values of wear‐scar diameter at higher loads and higher values of weld load in the four‐ball test than the lithium‐based grease alone. The prepared greases also passed rust and corrosion, and oxidation tests.     

复合组分对复合磺酸钙基润滑脂摩擦磨损性能的影响

制备4种不同组分的复合磺酸钙基润滑脂,采用四球摩擦磨损机和SVR高频线性振动试验机,考察12-羟基硬脂酸钙、硼酸钙对复合磺酸钙基润滑脂摩擦磨损性能的影响,采用XPS分析钢球磨斑表面主要元素的化学状态。结果表明,复合磺酸钙基润滑脂优良的极压性主要来源于层状结构的方解型碳酸钙沉积膜,而不是FeS、CaS、Fe3C、CaC2反应膜;抗磨性归功于硼酸钙、12-羟基硬脂酸钙所形成的极性吸附膜。     

Impact of polyurea structure on grease properties

The thickener structure of polyurea grease has a crucial effect on its properties. Therefore, it is very important to study the relationship between a thickener structure and physical and performance properties. In this study, polyurea greases were synthesised, having a different number of urea groups in per polyurea thickener molecule. Properties such as dropping point, penetration, oil separation, shear stability and four‐ball wear and extreme pressure (EP) were evaluated. The result shows that properties of polyurea grease vary with the number of urea group per polyurea molecule. Based on molecular theory, the mechanisms explaining these effects are briefly discussed. Copyright © 2010 John Wiley & Sons, Ltd.     

Influence of oil polarity and material combination on the tribological response of greases formulated with biodegradable oils and bentonite and highly dispersed silica acid

Different biodegradable lubricating greases formulated with esters of fatty acids, as base oils, and bentonite and highly dispersed silica acid, as thickener agents, were tribologically investigated in a nanotribometer and compared with polyalpha olefin greases with equal thickeners. Material combinations of steel ball on steel disc and sapphire ball on steel disc were used with different normal loads. Several friction and wear effects were found depending on the thickener and the base oil. The influence of grease components is also different in both material combinations evaluated. On the one hand, the base oil exerts a much higher impact on friction and wear in grease systems thickened with highly dispersed silica acid than in those thickened with bentonite. On the other hand, the latter reacts more sensitively to a change in material combination. Results were discussed and explained on the basis of polarity influences of the base oils and solid surfaces. Copyright © 2012 John Wiley & Sons, Ltd.     

The Friction Reducing Properties of Molybdenum Dialkyldithiocarbamate Additives: Part I — Factors Influencing Friction Reduction

Abstract

Calcium sulfonate complex greases have excellent extreme pressure, antiwear, and anticorrosion properties and are widely applied in rolling bearings, particularly in humid environments. In this article, the shear stability of dry and water-contaminated lubricating calcium sulfonate complex greases is described using a novel aging method. Unlike lithium and polyurea greases, no shear softening is observed for the dry greases due to the good mechanical stability of the particle-like thickener structure. For water-contaminated greases, no water separation was found during the prolonged aging. Instead, a homogeneous water–calcium sulfonate thickener micellar structure is generated. These micelles function as apparent thickeners and effectively increase the thickener concentration, which thickens the grease. This may explain why calcium sulfonate complex grease has excellent water absorption properties.     

Physical and chemical mechanisms of influence of Cu-containing additives on grease properties

The mechanisms governing the influence of copper additives (powders, oxides, organic and inorganic salts, complex compounds) on tribological, rheological and basic physical properties of greases with various thickeners (lithium, complex lithium, complex aluminium and polyurea) are discussed. The copper plating effect was found to occur only under EP conditions. The physical and chemical patterns of copper-containing grease additives under antiwear and extreme pressure conditions are discussed together with rational application alternatives in friction couples of equipment and machinery.     

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.     

Comparative study of the tribological properties of ionic liquids as additives of the attapulgite and bentone greases

Three kinds of ionic liquids (1‐butyl‐3‐methylimidazolium hexafluorophosphate (L‐P104), 1‐hexyl‐3‐methyl imidazolium hexafluorophosphate (L‐P106) and 1‐octyl‐3‐methylimidazolium tetrafluoroborate (LB108)) were added to the attapulgite base grease and the bentone base grease to investigate and compare the tribological behaviours of the ionic liquids with the two base greases at room temperature and 150°C. Tribological tests were performed using a ball‐on‐plate reciprocating tribometer. The attapulgite base grease showed better wear resistance properties than that of bentone base grease by adding ionic liquids as additives. At same time, the attapulgite base grease showed excellent friction‐reducing and wear resistance properties at high temperature (150°C). Also, we discussed the tribological mechanism of the attapulgite base grease at both room temperature and 150°C from the aspect of the structure of the grease thicker. Copyright © 2012 John Wiley & Sons, Ltd.     

Frictional performance of lithium 12‐hydroxystearate greases with different soap fibre structures in sliding contacts

The effect of the fibre structure of the grease on the frictional performance of lithium 12‐hydroxystearate greases with different fibre lengths was investigated in face, line, and point contact sliding tests. At high sliding speeds where the lubrication regime was practically hydrodynamic, the coefficient of friction of the base oil alone was lower than that of the greases. The coefficient of friction was roughly estimated as follows: base oil < long‐fibre grease < medium‐fibre grease < short‐fibre grease. The supply or replenishing capability of the grease played a critical role in maintaining hydrodynamic lubrication. At high contact pressures, the short‐fibre grease was superior in frictional performance to the long‐fibre grease due to the firm fibre network structure of the latter. In mixed and boundary lubrication regimes, the greases were superior in frictional performance to the base oil, since the soap fibres of the greases had a superior load‐carrying capacity. The long‐fibre grease, with a firm fibre structure, offered better frictional performance than the short‐fibre one.     

Rolling Bearing Performance and Film Formation Behavior of Four Multiply Alkylated Cyclopentane (MAC) Base Greases for Space Applications

Four multiply alkylated cyclopentane (MAC)-based greases, used for space applications, were used for rolling contact fatigue tests employing thrust ball bearings. These greases were R2000, ML, MU, and 5200 and were made from the same base oil 2001A. Each grease had a different thickener, which were sodium soap, Li soap, urea, and polytetrafluoroethylene (PTFE), respectively. The effect of the grease thickener on the ball bearings' fatigue life in vacuum and atmospheric environments was investigated via testing. For the greases R2000, MU, and ML it was found that the oil film formation in the experiments performed under vacuum conditions declined remarkably in comparison to under atmospheric conditions. For the 5200 grease, the oil film formation was almost the same as under atmospheric conditions. These results were supported by the occurrence of cage wear in the ball bearing fatigue tests. In the absence of sufficient films, high wear rates were measured.     

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.     

EP/AW performance evaluation of some zinc alkyl/dialkyl/alkylaryl‐dithiocarbamates in four‐ball tests

Tribochemistry, the chemistry of interacting surfaces under the influence of a lubricant, helps in the appropriate selection of suitable lubricant additives for specific uses. Modern lubricants are usually formulated from a range of petroleum base oils or synthetic fluids incorporating a variety of chemical additives for performance enhancement. Extreme‐pressure (EP) and anti‐wear (AW) additives are used extensively in lubricants for hypoid gears and metal cutting and forming operations to reduce wear, modify friction, and prevent scuffing of moving metallic parts. The present paper includes the synthesis and the evaluation of the tribological properties of 0.5% (w/v) solutions of some zinc bis‐(alkyl/dialkyl/alkylaryldithiocarbamates) in paraffin oil using 12.7 mm diameter steel bearing ball specimens in four‐ball tests. All the synthesised zinc dithiocarbamate additives in general, and zinc bis‐(morpholinodithio‐carbamate) (A₄) in particular, exhibited good AW, EP, and friction‐reducing properties. Additive A₄ especially gave low values of wear‐scar diameter and coefficient of friction at higher loads and higher values of load wear index and flash temperature parameter during EP tests (ASTM D 2783) and afforded lower values of wear‐scar diameter in a one‐hour wear test (ASTM D 2266–67). The surface topography of the wear‐scar matrix of the used ball specimens was investigated by scanning electron microscopy.     

Role of MoS2 morphology on wear and friction under spectrum loading conditions

One of the ways by which grease is evaluated is by using a four‐ball wear test using ASTM D2266. However, actual applications may require bearings to be subjected to spectrum loading conditions. This study focuses on using ball milling to mitigate the wear from sharp edges in the MoS₂ particles. Two different blends of greases were formulated using MoS₂ in the as‐received state (unmilled) and milled MoS₂; they were tested under spectrum loading conditions where the load and frequency of the tests were treated as variables. It was found that ball milling of the MoS₂ significantly reduces the wear under spectrum loading condition both for ramp‐up and ramp‐down conditions. It was also shown that shortening the time step for both the ramp‐up and ramp‐down cycles resulted in larger wear for unmilled MoS₂ particles in comparison with milled MoS₂ particles in grease. The milling process did not play a significant role when frequency of the test was either ramped up or down. 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.     

The Importance of Variable Speeds under Extreme Pressure Loading in Molybdenum Disulfide Greases Using Four-Ball Wear Tests

There is recent concern regarding grease behavior in extreme pressure applications. The research described here is aimed at providing good friction and wear performance while optimizing rotational speeds under extreme loading conditions. A design of experiment (DOE) was used to analyze molybdenum disulfide (MoS₂) greases and their importance in reducing wear under extreme loading and various speeds conditions (schedule 1 and schedule 2 speeds). The lamellar structure of MoS₂ provides very good weld protection by forming a layer that can be easily sheared under the applications of extreme pressures. An extreme load of 785 N was used in conjunction with different schedules of various rotational speeds to examine lithium-based grease with and without MoS₂ for an equal number of revolutions. A four-ball wear tester was utilized to run a large number of experiments randomly selected by the DOE software. The grease was heated to 75°C and the wear scar diameters were collected at the end of each test.

The results indicated that wear was largely dependent on the speed condition under extreme pressure loading, and thus a lower MoS₂ concentration is needed to improve the wear resistance of lithium-based greases. The response surface diagram showed that the developed molybdenum disulfide greases exhibited both extreme pressure as well as good wear properties under various rotational speeds when compared to steady-state speed. It is believed that MoS₂ greases under schedule 1 speeds perform better and provide an antiwear film that can resist extreme pressure loadings.     

The properties of various antiwear and extreme‐pressure additives in pentaerythritol ester

The tribological properties of three representative antiwear and extreme‐pressure additives, tricresylphosphate (TCP), triphenylthiophosphate (TPPT), and α‐mercaptobenzothiazole (MBT), in pentaerythritol ester at different concentrations were studied. It was found that TCP could react with Fe to form an organic phosphate film containing 4% P on the scar surface, while TPPT formed a blended organic phosphate and inorganic FeS film, containing 4% P and 6% S, respectively. MBT formed an inorganic FeS film containing 45% S. Ferrographic analyses of wear particles collected from oil samples after four‐ball tests showed that the higher the temperature the better the tribological performance of the additivated ester, due to its reaction with the metal surface.     

Studies of the Synthesis and Utilisation of Schiff's Bases: I. Schiff's Bases as Antioxidants for Lubricating Greases

Three Schiff's bases have been prepared as antioxidants for three grades of lubricating grease. The following Schiff's base compounds were synthesised: 3‐[(p‐chlorophenyl)iminomethylenyl]‐4‐hydroxy‐8‐methyl‐2(1H)‐quinolinone and its bromo and iodo analogues. The structures of these compounds have been confirmed using elemental analysis, nuclear magnetic resonance, and infrared spectroscopy. The quinolinone compounds were added to the lubricating greases in different concentrations. The antioxidant efficiency of these bases have been determined using infrared spectroscopy and total acid number. The results indicate that the oxidation stability of the lubricating greases is affected by the type of fatty acid they contain. It was found that the three types of grease resist oxidation in the presence of the Schiff's bases; the efficiency of these compounds as antioxidants decreases in the order: p‐chloro > p‐bromo > p‐iodo derivative. The mechanisms of operation of the quinolinone derivatives as scavengers for free radicals are suggested.     

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。     

极压抗磨添加剂在复合锂基润滑脂中作用的研究

将3种极压抗磨添加剂(T304、T321和T404)分别加入到4种不同组分的复合锂基润滑脂中,考察其对润滑脂性能的影响。研究发现,加入不同的添加剂后润滑脂的油膜强度增加,锥入度增大,滴点降低;在添加同样剂量的情况下,T304和T321对复合锂基润滑脂的油膜强度影响较大;T321和T404对复合锂基润滑脂的锥入度影响较大;T304和T321对复合锂基润滑脂的滴点影响较大。并对其作用机制进行了分析,认为是由于极压抗磨添加剂分子中带负电性的双键和带正诱导效应及空间位阻效应的支链共同作用的结果。