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

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Abstract

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.

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References

  1. Czarny, R.: Lubricating greases (in Polish). Wydawnictwo Naukowo-Techniczne, Warsaw (2004)

    Google Scholar 

  2. Paszkowski, M., Olsztyńska-Janus, S.: Grease thixotropy: evaluation of grease microstructure change due to shear and relaxation. Ind. Lub. Tribol. 2(66), 223–237 (2014)

    Article  Google Scholar 

  3. Czarny, R.: Lubrication of the wheels and suspension of engineering machines and vehicles (in Polish). Wroclaw University of Technology Publishing House, Wroclaw (1998)

    Google Scholar 

  4. Biernacki, K.: An analysis of the phenomena taking place in the boundary layer of a lubricating grease (in Polish). Tribology: friction, wear, lubrication. 5, 111–129 (2006)

  5. Biernacki, K.: The influence of the kind of wall material, shear rate and temperature on the shearing stress value in lubricating greases (in Polish). Tribology: friction, wear, lubrication. 6, 75–85 (2007)

  6. Czarny, R., Paszkowski, M.: The influence of graphite solid additives, MoS2 and PTFE on changes in shear stress values in lubricating greases. J. Syn. Lub. 24, 19–29 (2007)

    Article  Google Scholar 

  7. Czarny, R.: A method for the determination of the yield stress in greases. World Tribology Congress. Vienna, Italy (2001)

    Google Scholar 

  8. Lugt, P.: Grease lubrication in rolling bearings. Willey, Chichester (2013)

    Google Scholar 

  9. Paszkowski, M.: Identification of the thixotropy of lithium greases, 16th International Colloquium Tribology 2008—Lubricants, Materials and Lubrication Engineering. Stuttgart/Ostfildern, Germany (2008)

  10. Paszkowski, M.: Some aspects of grease flow in lubrication systems and friction nodes. In: Gegner, J. (ed.) Tribology—fundamentals and advancements, pp. 77–106. InTech, Rijeka (2013)

    Google Scholar 

  11. Paszkowski, M.: Assessment of the effect of temperature, shear rate and thickener content on the thixotropy of lithium lubricating greases. Proc. Inst. Mech. Eng. J.—J. Eng. Tribol. 3, 209–219 (2013)

    Article  Google Scholar 

  12. Olsztyńska-Janus, S.: Attenuated total reflectance (ATR) method (in Polish). In: Komorowski, L., Olszowski, A. (eds.) Physical chemistry, vol. 4, physicochemical laboratory, pp. 214–217. PWN, Warsaw (2013)

    Google Scholar 

  13. Olsztyńska-Janus, S., Gąsior-Głogowska, M., Szymborska-Małek, K., Walski, T., Komorowska, M., Witkiewicz, W., Pezowicz, C., Kobielarz, M., Szotek, S.: Spectroscopic techniques in the study of soft tissues and their components. Part I: IR spectroscopy. Acta Bioeng. Biomech. 14(3), 101–115 (2012)

    Google Scholar 

  14. Olsztyńska-Janus, S., Gąsior-Głogowska, M., Szymborska-Małek, K., Czarnik-Matusewicz, B., Komorowska, M.: Specific applications of vibrational spectroscopy. In: Komorowska, M., Olsztyńska-Janus, S. (eds.) Biomedical engineering, trends, research and technologies, pp. 91–120. InTech, Rijeka (2011)

    Chapter  Google Scholar 

  15. ASTM Standard D217-10: Standard test methods for cone penetration of lubricating grease (2010)

  16. Shih, W.H., Shih, W.Y., Kim, S.I., Liu, J., Aksay, I.A.: Scaling behaviour of the elastic properties of colloidal gels. Phys. Rev. A 42, 4772–4779 (1990)

    Article  Google Scholar 

  17. Yeong, S.K., Luckham, P.F., Tadros, ThF: Steady flow and viscoelastic properties of lubricating grease containing various thickener concentrations. J. Colloid Interf. Sci. 274, 285–293 (2004)

    Article  Google Scholar 

  18. Martín-Alfonso, J.E., Moreno, G., Valencia, C., Sánchez, M.C., Franco, J.M., Gallegos, C.: Influence of soap/polymer concentration ratio on the rheological properties of lithium lubricating greases modified with virgin LDPE. J. Ind. Eng. Chem. 5, 687–693 (2009)

    Article  Google Scholar 

  19. Franco, J.M., Delgado, M.A., Valencia, C., Sánchez, M.C., Gallegos, C.: Mixing rheometry for studying the manufacture of lubricating greases. Chem. Eng. Sci. 60, 2409–2418 (2005)

    Article  Google Scholar 

  20. Delgado, M.A., Valencia, C., Sánchez, M.C., Franco, J.M., Gallegos, C.: Thermorheological behaviour of a lithium lubricating grease. Tribol. Lett. 23, 47–54 (2006)

    Article  Google Scholar 

  21. Sánchez, M.C., Franco, J.M., Valencia, C., Gallegos, C., Urquiola, F., Urchegui, R.: Atomic force microscopy and thermo-rheological characterisation of lubricating greases. Tribol. Lett. 41, 463–470 (2011)

    Article  Google Scholar 

  22. Fahrenfort, J.: Attenuated total reflection: a new principle for the production of useful infra-red reflection spectra of organic compounds. Spectrochim. Acta 17(7), 698–709 (1961)

    Article  Google Scholar 

  23. Olsztyńska-Janus, S.: Vibrational spectrum (in Polish). In: Komorowski, L., Olszowski, A. (eds.) Physical chemistry, vol. 4, physicochemical laboratory, pp. 669–679. PWN, Warsaw (2013)

    Google Scholar 

  24. Olsztyńska-Janus, S., Komorowska, M.: Conformational changes of l-phenylalanine induced by near infrared radiation ATR–FTIR studies. Struct. Chem. 23, 1399–1407 (2012)

    Article  Google Scholar 

  25. Tadros, FTh: Rheology of dispersions: principles and applications. Wiley, Weinheim (2010)

    Book  Google Scholar 

  26. Tadros, FTh: Use of viscoelastic measurements in studying interactions in concentrated dispersions. Langumir 6, 28–35 (1990)

    Article  Google Scholar 

  27. Sokrates, G.: Infrared characteristic group frequencies. Tables and charts. Wiley, New York (1994)

    Google Scholar 

  28. Olsztyńska-Janus, S.: Infrared spectrum and Raman spectrum (in Polish). In: Komorowski, L., Olszowski, A. (eds.) Physical Chemistry, vol. 4, Physicochemical laboratory, pp. 670–674. PWN, Warsaw (2013)

    Google Scholar 

  29. Olsztyńska-Janus, S., Dupuy, N., Vrielynck, L., Komorowska, M.: Water evaporation analysis of l-phenylalanine from initial aqueous solutions to powder state by vibrational spectroscopy. Appl. Spectrosc. 60, 1040–1053 (2006)

    Article  Google Scholar 

  30. Cann, P.M.: Grease degradation in R0F bearing tests. Tribol. T. 50, 187–197 (2007)

    Article  Google Scholar 

  31. Cann, P.M.: Grease degradation in a bearing simulation device. Tribol. Int. 39, 1698–1706 (2006)

    Article  Google Scholar 

  32. Guillén, M.D., Cabo, N.: Infrared spectroscopy in the study of edible oils and fats. J. Sci. Food Agric. 75, 1–11 (1997)

    Article  Google Scholar 

Download references

Acknowledgments

Some results of this research were presented at the 5th World Tribology Congress, Torino, Italy, September 8–13, 2013. The research was funded by the Institute of Machine Design and Operation and the Institute of Biomedical Engineering and Instrumentation, at Wroclaw University of Technology. Wroclaw, Poland. The Golden Gate Mk II ATR Accessory with Heated Diamond Top-plate (USA), purchased with funds provided as part of the grant “Equipment for the Community Biooptics Laboratory in the Institute of Biomedical Engineering and Instrumentation at Wroclaw University of Technology” No. 6180/IA/119/2012 by the Ministry of Science and Higher Education, was used in the studies. The authors would like to give their heartfelt thanks to Prof. Małgorzata Komorowska from the Institute of Biomedical Engineering and Instrumentation at Wroclaw University of Technology for the fruitful discussion and Dr. Anna Zajezierska from the Oil and Gas Institute in Cracow for preparing the grease sample for the tests.

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Authors and Affiliations

  1. Institute of Machine Design and Operation, Wroclaw University of Technology, Ignacego Lukasiewicza 7/9, 50-371, Wroclaw, Poland

    Maciej Paszkowski

  2. Institute of Biomedical Engineering and Instrumentation, Wroclaw University of Technology, Plac Grunwaldzki 13, 50-370, Wroclaw, Poland

    Sylwia Olsztyńska-Janus & Iwona Wilk

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  1. Maciej Paszkowski
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  2. Sylwia Olsztyńska-Janus
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  3. Iwona Wilk
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Correspondence to Maciej Paszkowski.

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Paszkowski, M., Olsztyńska-Janus, S. & Wilk, I. Studies of the Kinetics of Lithium Grease Microstructure Regeneration by Means of Dynamic Oscillatory Rheological Tests and FTIR–ATR Spectroscopy. Tribol Lett 56, 107–117 (2014). https://doi.org/10.1007/s11249-014-0390-4

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  • DOI: https://doi.org/10.1007/s11249-014-0390-4

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