Grease Microstructure Research Articles

On the Optical Assessment of the Structural Degradation of Rheologically Stressed Lubricating Greases

This work explores optical measurements' potential to better understand structural degradation due to the internal friction process of lubricating greases. The samples have been examined as closely as possible to their original state due to the specimen preparation protocol. Eleven model lubricating greases were evaluated for these purposes. Image analysis of transmitted light microscope, SEM and AFM measurements were used to evaluate the grease microstructure under stressed and unperturbed conditions. The results showed that the type of thickener could significantly influence the internal frictional energy due to the structural degradation of the lubricating grease. Thus, the structural skeletons of lithium and calcium greases can dissipate less mechanical energy during a shearing process than polyurea grease or isolated pure biogenic greases.

Microstructure Characterization of Degraded Grease in Axle Roller Bearings

Aged mineral-oil-based, lithium-hydroxystearate-thickened grease was collected from used axle spherical roller bearings, which were used for urban commuter trains. Three types of aged grease were categorized based on the total distance that the bearing had traveled, as early life (<0.05 million km [M.km]), medium (0.3–0.6 M.km), and heavily used (1.82 and 2.0 M.km). The microstructure of degraded grease from 20 bearings was characterized in this project using atomic force microscopy (AFM) and scanning electron microscopy (SEM). Base oil of each grease sample was released by a centrifugation method and the oxidation of bled oil was measured by infrared analysis. A notable change in grease microstructure was observed by AFM and SEM. The thickener morphology changed from an entangled helical fibril structure to particle-like nanofragments. The variation in thickener microstructure was observed in the early life grease, which suggested grease can experience an inconsistent aging process in the real-life bearings. Overall, 70.5 ± 1.37 wt% base oil bled from the fresh grease, 68.2 ± 0.73 wt% from the early life grease, 58.1 ± 2.33 wt% from the medium used grease, and 60.0 ± 6.35 wt% from the heavily used grease. The results suggest that the densely packed microstructure observed in the aged grease affects the capability of base oil bleeding from the grease. The retardation of base oil flow due to degraded grease may result in the lubricating ability of grease becoming compromised and hence result in an increased wear rate of the bearings.

Novel polymer grease microstructure and its proposed lubrication mechanism in rolling/sliding contacts

A novel polymer grease micro-structure is revealed using scanning electron microscopy (SEM), cryogenic scanning electron microscopy (cryo-SEM) and transmission electron microscopy (TEM). The structure consists of amorphous polypropylene nano-particles uniformly distributed in the base oil. This novel microstructure has never been documented before. Rheology shows that there is no irreversible shear-thinning. The grease shows excellent stability and flow behaviours. In the absence of crystallization and a network thickener structure, it has a potential for use at extremely low start-up temperatures. Spherical roller bearing (SRB) testing shows excellent lubricating performance and the potential for lowering friction in comparison with benchmark greases. It is hypothesized that the grease behaves as a highly stable nano-fluid allowing abundant oil replenishment into the rolling contact, whereby nanoparticles are released with the base oil in the contact.

Studies of the Kinetics of Lithium Grease Microstructure Regeneration by Means of Dynamic Oscillatory Rheological Tests and FTIR–ATR Spectroscopy

As part of this research, the kinetics of soap grease thickener microstructure regeneration during 24-h relaxation after 1-h shearing were studied. A lubricating grease, based on mineral oil ORLEN OIL SN-400, containing associated molecules of lithium 12-hydroxystearate was subjected to analysis. Rheological dynamic oscillatory and FTIR–ATR (Fourier Transform Infrared Attenuated Total Reflectance) spectroscopy were used to study the kinetics of thickener microstructure regeneration. Changes in the values of storage modulus G′ and loss modulus G″ of the investigated grease during its relaxation in the linear viscoelastic range were examined. In addition, the mechanical stability of the thickener microstructure at a variable oscillation frequency was tested, and changes in the cohesive energy of the grease versus the latter’s relaxation time were assessed. FTIR–ATR spectroscopy was used to study the physicochemical interactions between the associated molecules of lithium 12-hydroxystearate. Infrared bands were assigned to the vibrations of the particular functional groups of the grease components, and the spectral parameters in the absorption spectra in the range of 700–3,700 cm−1 were examined. The studies carried out using the two investigative methods have revealed that the intensity of thickener microstructure regeneration was the highest in the first hour of grease relaxation after shearing. In this time interval, the largest changes in the vibrations of the main functional groups of the grease components were observed. In the next hours, the kinetics of thickener microstructure regeneration were substantially lower.

Grease thixotropy: evaluation of grease microstructure change due to shear and relaxation

Purpose – The thixotropy of lubricating grease thickened with lithium 12-hydroxystearate with mineral base oil was investigated. The thixotropy has a significant influence on the flow resistance and pressure drop in the structural components of lubrication systems, which is of major importance as today the latter are being centralized and automated. The paper aims to discuss these issues. Design/methodology/approach – Rheometer studies on thixotropy were carried out and the grease microstructure was visualized using atomic force microscopy (AFM). Total reflection Fourier transform infrared spectroscopy (ATR-FTIR) was used to study the physicochemical interactions which indicate the disintegration and recovery of the grease microstructure. Findings – A qualitative assessment of the physicochemical interactions between lithium soap floccules was made and a theory of the self-ordering effect of lithium 12-hydroxystearate associated molecules during shearing and their aggregation and flocculation during relaxation has been proposed. Originality/value – Because of the complexity of the disintegration and recovery of the lubricating grease thickener microstructure, there is still limited physical understanding of the mechanism of this process. Therefore, the present research was undertaken to identify the phenomena involved.

Assessment of the effect of temperature, shear rate and thickener content on the thixotropy of lithium lubricating greases

As part of this research the thixotropy of lubricating greases based on mineral oil ORLEN OIL SN-400, thickened with lithium 12-hydroxystearate has been investigated. The investigations consisted in shearing grease samples in the rotational rheometer head for 1 h, followed by 24- h relaxation and again 1-h shearing, at a constant shear rate gradient. The increase in the structural viscosity of the grease, caused by the partial reconstruction of the lithium thickener microstructure between the two shearing stages, after 24- h relaxation, was studied. The studies have shown that there is a non-unique dependence between grease temperature T, shear rate gradient [Formula: see text], thickener percentage Sc and the intensity of grease microstructure reconstruction. In the adopted ranges of the input quantities: T (from −20 °C to + 80 °C), [Formula: see text] (from 8.1 to 48.6 s−1) and Sc (from 4% to 9%), the largest increment in structural viscosity was observed for the grease with thickener percentage Sc = 7.5%, sheared at shear rate gradient [Formula: see text] = 8.1 s−1 at temperature T = 28 °C. On the basis of the experimental studies, a mathematical relation for predicting the increment in the structural viscosity of lithium greases in different shearing conditions has been developed. The relation can find wide application in engineering practice in the design of machine lubrication systems and in the selection of lubricating media thickened with lithium soap.

Atomic Force Microscopy and Thermo-Rheological Characterisation of Lubricating Greases

In this work, non-perturbed microstructures of several commercial and model lubricating greases, differing in nature and concentration of the thickener agent, were examined using the atomic force microscopy (AFM) technique. Grease microstructure mainly depends on the nature of the thickener employed and, also, on thickener concentration and viscosity of the base oil. Thermal-induced changes in the viscoelastic response of lubricating greases have been investigated by using different rheological techniques in a temperature range of 0–175 °C. Small-amplitude oscillatory shear (SAOS) measurements were carried out to determine the mechanical spectra of the different samples studied. Lubricating grease rheological thermal susceptibility was analysed by following the evolution of the plateau modulus with temperature. SAOS functions dramatically decrease, in most cases, above a characteristic temperature, which depends on nature and/or concentration of the thickener used and therefore on grease microstructure. The thermo-mechanical reversibility of grease microstructure has been studied by carrying out triple-step-shear stress tests (shear stresses inside and outside of the linear viscoelasticity range), at different temperatures. The degree of lubricating grease non-reversible structural breakdown, which increases with temperature, depends on the shear stress applied above the linear viscoelasticity limits.

Influence of soap/polymer concentration ratio on the rheological properties of lithium lubricating greases modified with virgin LDPE

The main goal of this work was to study the feasibility of using a low-density polyethylene (LDPE) as additive to improve the rheological properties of lithium lubricating greases. The combined effect that both soap and LDPE concentrations exerts on the rheology of lithium lubricating greases and its relationship with grease microstructure were studied according to an experimental design based on the response surface methodology (RSM). Different lubricating grease formulations were manufactured by modifying lithium 12-hydroxystereate and LDPE concentrations. Small-amplitude oscillatory shear (SAOS) and viscous flow measurements, as well as mechanical stability tests, were performed. In addition to these, environmental scanning electronic microscopy (ESEM) was used to determine grease microstructure. LDPE was found to be a useful additive to modify grease rheology, acting as filler in the entangled soap network. The values of both apparent viscosity and linear viscoelasticity functions increase with soap and LDPE concentration. However, the addition of LDPE distorts soap microstructural network, yielding greases with lower relative elastic characteristics.

Transient shear flow of model lithium lubricating greases

This paper deals with the analysis of the transient shear flow behavior of lithium lubricating greases differing in soap concentration and base oil viscosity. The shear-induced evolution of grease microstructure has been studied by means of stress-growth experiments. With this aim, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and the viscosity of the base oil, according to a RSM statistical design. Moreover, atomic force microscopy (AFM) observations were carried out. The transient stress response can be successfully described by the generalized Leider-Bird model based on two exponential terms. Different rheological parameters, related to both the elastic response and the structural breakdown of greases, have been analysed. In this sense, it has been found that the elastic properties of lithium lubricating greases were highly influenced by soap concentration and oil viscosity. The stress overshoot, τ max , depends linearly on both variables in the whole shear rate range studied, although the effect of base oil viscosity on this parameter is opposite at low and high shear rates. Special attention has been given to the first part of the stress-growth curve. In this sense, it can be deduced that the “yielding” energy density not only depends on grease composition, but also on shear rate. Moreover, an interesting asymptotic tendency has been found for both the “yielding” energy density and the stress overshoot by increasing shear rate. The asymptotic values of these parameters have been correlated to the friction coefficient obtained in a ball-disc tribometer.

Drainage-Induced Dry-Out of Thermal Greases

In this study, the mechanism of grease dry-out, a long-term failure mode of thermal greases, is investigated using optical microscopy and infrared (IR) thermography. Results show that the dry-out phenomenon is accelerated in aged greases and we suggest that this is due to inhomogeneities in the filler packing structure that develop over time due to segregation of the grease components, though they may also occur at time zero due to insufficient mixing during grease formulation. Theories describing fluid flow through porous media are used as a preliminary framework for understanding the grease dry-out process and its dependence on local variations in the grease microstructure and on matrix-filler compatibility.

Recycled and virgin LDPE as rheology modifiers of lithium lubricating greases: A comparative study

AbstractIn this work, a new application for recycled low‐density polyethylene (LDPE), as rheology modifier of standard lithium lubricating grease formulations, was studied. The effectiveness of this additive was compared with that achieved with a virgin LDPE. With this aim, both types of polymers were added to the formulation during the manufacturing process of greases, following the same standard protocol, to reinforce the role of the thickening agent, the lithium 12‐hidroxystearate. The effect that both lithium soap and LDPE concentrations exert on the rheology of lubricating grease formulations and its relationship with grease microstructure were discussed. Lubricating greases were rheologically characterized through small‐amplitude oscillatory shear and viscous flow measurements. In addition to these, scanning electron microscopy observations and mechanical stability tests were also carried out. In all cases, an increase in soap concentration yields higher values of apparent viscosity and linear viscoelasticity functions. On the other hand, the values of the rheological functions obtained for recycled LDPE‐based lubricating greases are, in general, higher than those obtained for virgin LDPE‐based grease formulations. However, the structural skeleton developed in greases containing recycled LDPE demonstrates less resistance to severe working conditions, showing lower mechanical stability than virgin LDPE‐based grease formulations. POLYM. ENG. SCI., 2008. © 2008 Society of Plastics Engineers

Development of new lubricating grease formulations using recycled LDPE as rheology modifier additive

The recovery of plastic waste but also its applicability in product development may be an incentive to industry, since the use of such plastics represents a cheaper source of raw material. The aim of the present paper is to study the feasibility of recycling polyolefins as additives to improve the rheological properties of lithium 12-hydroxystearate lubricating greases. The effects that both soap and recycled low-density polyethylene (LDPE) concentration exert on the rheology of lithium lubricating greases and its relationship with grease microstructure are discussed in this work. In this way, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and content of recycled LDPE, according to a RSM statistical design. These lubricating greases were rheologically characterized through small-amplitude oscillatory shear (SAOS) and viscous flow measurements. In addition to these, scanning electronic microscopy (SEM) observations and mechanical stability tests were also carried out. Recycled LDPE was found to be an effective additive to modify grease rheology, acting as filler in the soap entangled microstructure. The values of both apparent viscosity and viscoelastic functions in the linear viscoelastic region increase with soap and recycled polymer concentrations. However, the addition of recycled LDPE distort the microstructural network of these greases resulting greases with less relative elastic characteristics and poorer mechanical properties as LDPE content increases.

Thermorheological behaviour of a lithium lubricating grease

Thermal-induced changes in the viscous and viscoelastic responses of lubricating greases have been investigated through different rheological techniques in a temperature range of 0–175 °C. Small-amplitude oscillatory shear and viscous flow measurements were carried out on a model conventional lithium lubricating grease prepared by inducing the in situ saponification reaction between 12-hydroxystearic acid and hydrated lithium hydroxide. The linear viscoelasticity functions dramatically decrease above 110 °C, but not below this critical temperature, which determines the maximum recommended operating temperature in relation to its durability and resistance under working conditions. Two different regions, below and above this critical temperature, in the plateau modulus versus temperature plot have been detected. From this thermal dependence, a much larger thermal susceptibility of the lubricating grease at temperatures above 110 °C is apparent. The thermo-mechanical reversibility of this material has been studied by applying different combined stress–temperature protocols. Regarding the viscous flow, a minimum in the shear stress versus shear rate plots appeared at temperatures above 60 °C, more pronounced as temperature increases, resulting from material instabilities. The experimental results obtained have been explained on the basis of the thermo-mechanical degradation of the lubricating grease microstructure.

Influence of Soap Concentration and Oil Viscosity on the Rheology and Microstructure of Lubricating Greases

The effects that both soap concentration and base oil viscosity exert on the rheology of lubricating greases and its relationship with grease microstructure are discussed in this work. With this aim, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and the viscosity of the base oil, according to an RSM statistical design. These lubricating greases were rheologically characterized through small-amplitude oscillatory shear (SAOS) and viscous flow measurements. In addition to these, scanning electronic microscopy (SEM) observations and mechanical stability tests were also carried out. It has been found that the structural skeleton (size and shape of the disperse phase particles) was highly influenced by the base oil viscosity. In this sense, the values of the viscoelastic functions in the linear viscoelastic region and the mechanical stability of the lubricating greases increase as the viscosity of the base oil decreases. An opposite ten...

Fatty acids and antioxidant effects on grease microstructures

The search for biobased material as industrial and automotive lubricants has accelerated in recent years. This trend is primarily due to the nontoxic and biodegradable characteristics of seed oils that can substitute mineral oil as base fluid in grease making. The paper discusses the preparation of lithium soap-based soy greases using different fatty acids and the determination of crystallite structure of soap using transmission electron microscopy (TEM). Lithium soaps with palmitic, stearic, oleic, and linoleic acids were synthesized and mixed with soybean oil (SBO) and additives to obtain different grease compositions. TEM measurements have revealed that the soap crystallite structure impact grease consistency. Soap fiber length and their cross-linking mechanism in the matrix control grease consistency (National Lubricating Grease Institute (NLGI) hardness, ASTM D-217 method). Lithium stearate-based soy grease has a relatively more compact fiber structure than Li palmitate. Linoleic acid (C 18,  ) with two sites of CC unsaturation in the chain has a much thinner and more compact fiber network than oleic acid (C 18, ). The presence of additive in grease produces a soap with looser network and larger fiber structure than similar grease containing no additive. A close analysis of grease microstructure will help in the development of better performing grease for industrial applications.

Rheology modifier

The recovery of plastic waste but also its applicability in product development may be an incentive to industry, since the use of such plastics represents a cheaper source of raw material. The aim of the present paper is to study the feasibility of recycling polyolefins as additives to improve the rheological properties of lithium 12-hydroxystearate lubricating greases. The effects that both soap and recycled low-density polyethylene (LDPE) concentration exert on the rheology of lithium lubricating greases and its relationship with grease microstructure are discussed in this work. In this way, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and content of recycled LDPE, according to a RSM statistical design. These lubricating greases were rheologically characterized through small-amplitude oscillatory shear (SAOS) and viscous flow measurements. In addition to these, scanning electronic microscopy (SEM) observations and mechanical stability tests were also carried out. Recycled LDPE was found to be an effective additive to modify grease rheology, acting as filler in the soap entangled microstructure. The values of both apparent viscosity and viscoelastic functions in the linear viscoelastic region increase with soap and recycled polymer concentrations. However, the addition of recycled LDPE distort the microstructural network of these greases resulting greases with less relative elastic characteristics and poorer mechanical properties as LDPE content increases.