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Surface-wetting characterization using contact-angle measurements

Nature Protocols volume 13, pages 1521–1538 (2018)Cite this article

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A Publisher Correction to this article was published on 07 August 2018

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Abstract

Wetting, the process of water interacting with a surface, is critical in our everyday lives and in many biological and technological systems. The contact angle is the angle at the interface where water, air and solid meet, and its value is a measure of how likely the surface is to be wetted by the water. Low contact-angle values demonstrate a tendency of the water to spread and adhere to the surface, whereas high contact-angle values show the surface’s tendency to repel water. The most common method for surface-wetting characterization is sessile-drop goniometry, due to its simplicity. The method determines the contact angle from the shape of the droplet and can be applied to a wide variety of materials, from biological surfaces to polymers, metals, ceramics, minerals and so on. The apparent simplicity of the method is misleading, however, and obtaining meaningful results requires minimization of random and systematic errors. This article provides a protocol for performing reliable and reproducible measurements of the advancing contact angle (ACA) and the receding contact angle (RCA) by slowly increasing and reducing the volume of a probe drop, respectively. One pair of  ACA and RCA measurements takes ~15–20 min to complete, whereas the whole protocol with repeat measurements may take ~1–2 h. This protocol focuses on using water as a probe liquid, and advice is given on how it can be modified for the use of other probe liquids.

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Fig. 1: A drop of water on an ideal solid substrate.
Fig. 2: Static water drops.
Fig. 3: Sketch of the Gibbs free energies of ideal and real wetting systems as a function of the apparent contact angle.
Fig. 4: Different stages of ACA and RCA measurement.
Fig. 5: Sketch of a goniometer setup.
Fig. 6: Recommended starting volume for RCA measurement, i.e., minimum advancing drop volume (Va) needed to reach RCA at 10 µL.
Fig. 7: Receding-contact-angle data of a nanostructured polysiloxane film on silicon substrate.
Fig. 8: Advancing contact-angle data of a nanostructured polysiloxane film on silicon substrate.
Fig. 9: Effect of advancing drop volume (Va) on the receding contact-angle measurement.
Fig. 10: Needle position for a very hydrophobic surface with low contact-angle hysteresis.

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Change history

  • 07 August 2018

    The version of this Protocol originally published contained typographical errors that affected the accuracy/readability of the text. In Fig. 4e, the line “Contact angle remainsstable” should have read “Contact angle remains stable.” In Table 1, in the “Advantages” column, the second instance of “Simple” was incorrectly associated with the “Sessile-drop goniometry” method; it should have corresponded to the “Tilting plate” method. In Table 2, in the “Issues” column, the entry “Difficult to place baseline when the RCA is ~90°” was broken incorrectly in a way that might have suggested that “the RCA is ~90°” was a separate issue. These errors have been corrected in the HTML and PDF versions of the paper.

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Acknowledgements

The protocol is the result of a procedure gradually developed since wetting research was begun in the R.H.A.R. group, and we acknowledge the contributions of H. Mertaniemi, T. Verho and M. Latikka. This work was supported by the European Research Council ERC-2016-CoG (725513-SuperRepel) and the Academy of Finland (Centres of Excellence Programme 2014–2019). X.T. is grateful for the support of the One Hundred Talents Program of SYSU and the One Thousand Youth Talents Program of China.

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Author notes

  1. Juuso T. Korhonen

    Present address: Department of Neuroscience and Biomedical Engineering, School of Science, Aalto University, Espoo, Finland

Authors and Affiliations

  1. Department of Applied Physics, School of Science, Aalto University, Espoo, Finland

    Tommi Huhtamäki, Xuelin Tian, Juuso T. Korhonen & Robin H. A. Ras

  2. School of Materials Science and Engineering, Sun Yat-sen University, Guangzhou, China

    Xuelin Tian

  3. Department of Bioproducts and Biosystems, School of Chemical Engineering, Aalto University, Espoo, Finland

    Robin H. A. Ras

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  1. Tommi Huhtamäki
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Contributions

R.H.A.R. coordinated the project. T.H., X.T. and J.T.K. performed the experiments. All authors participated in designing the protocol. T.H. and R.H.A.R. wrote the manuscript with contributions from all authors. J.T.K. wrote the Python code.

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Correspondence to Robin H. A. Ras.

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The authors declare no competing interests.

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Related links

Reliable measurement of the receding contact angle: https://doi.org/10.1021/la400009m

Guidelines to measurements of reproducible contact angles using a sessile-drop technique: https://doi.org/10.1680/si.13.00010

Characterization of super liquid-repellent surfaces: https://doi.org/10.1016/j.cocis.2014.04.009

Supplementary information

Supplementary Methods: Python code for solving the Young–Laplace equation.

The minimum advancing drop volumes (= the recommended starting volume for the receding contact-angle measurement) needed to reach RCA at 10 µL (Fig. 6), were obtained by solving the Young–Laplace equation by numerical integration, using Python programming language with Scipy library. The shape and size of the drop for different pairs of contact angle and drop volume were solved using a code that is provided in this supplementary file

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Huhtamäki, T., Tian, X., Korhonen, J.T. et al. Surface-wetting characterization using contact-angle measurements. Nat Protoc 13, 1521–1538 (2018). https://doi.org/10.1038/s41596-018-0003-z

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