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Ice-Templating: Processing Routes, Architectures, and Microstructures

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Freezing Colloids: Observations, Principles, Control, and Use

Part of the book series: Engineering Materials and Processes ((EMP))

Abstract

This chapter concentrates on materials science studies and applications of freezing colloids. Both porous and dense materials are obtained by freezing colloids; processes called ice-templating or freeze-casting in materials science. After a brief history of how the idea of ice-templating emerged after the initial observations of freezing-induced segregation more than a century ago, this chapter describes the processing routes developed to date. In particular, the combination of traditional materials processing routes with freezing provides materials with unique architectures and microstructures. The third section of the chapter presents the architectures and microstructures of ice-templated materials. As most of the freezing routes have been developed to obtain porous materials, we then go into details in the characteristics of the porosity at multiple levels, from macropores to meso- and micropores, as well as the different architectures obtained by freezing routes, including aerogels, fibres, or microparticles.

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Notes

  1. 1.

    Working on freezing was difficult at the beginning of the \(20^{th}\) century. Because of the absence of cooling devices, scientists had to rely on low temperatures encountered in winter. Taber performed a first series of observations at night, during the winter of 1914/1915. The following winter were apparently not cold enough for his freezing experiments, and he gave up on the investigations for 12 years, until he had access to a freezing device in his lab:

    Experiments carried out by me on cold nights during the winter of 1914–15 indicated that the pressure effects [...]. After publishing brief descriptions of some of these experiments together with certain conclusions, I laid the investigation aside temporarily, because of the lack of facilities for obtaining and maintaining low temperatures. In March 1927, suitable low-temperature apparatus was placed at my disposal [...] and I began an investigation to determine the factor involved in excessive and in differential frost heaving.

  2. 2.

    See p. 135 and after.

  3. 3.

    Starting from the same observations, Halberstadt and Henisch hypothesised a few years later [8] that “since there is no visible shrinkage [upon freeze drying], it is reasonable to assume that the gel structure remains intact”. This assumption turned out to be wrong. The gel structure was modified locally by the growth of the crystals, even if the overall dimensions of the sample remained the same.

  4. 4.

    See p. 154 for the mechanisms.

  5. 5.

    See p. 400.

  6. 6.

    See p. 400.

  7. 7.

    See p. 112 and p. 114.

  8. 8.

    See p. 386.

  9. 9.

    See p. 387.

  10. 10.

    These investigations were ground-based. The antenna used to measure the impulse reflections were placed 1 m above the ground .

  11. 11.

    See p. 389 and after.

  12. 12.

    See p. 365.

  13. 13.

    See p. 447.

  14. 14.

    These aspects are discussed p. 111.

  15. 15.

    P123 was also used obtained mesoporosity in titania [238]. Little indications are nevertheless given about the processing conditions, or the deliberate intentions to obtain micelles before or during freezing. The final product is a powder, not a bulk sample.

  16. 16.

    Given p. 448 (Chap. 7).

  17. 17.

    Of course, they did not refer to the process as freeze-casting or ice-templating at that time. They mentioned that the fibres are “occasionally branched, and seem to be the remnants of the ridged flakes where the interconnections between ridges have thinned to the vanishing point”. The figure of the flakes (Fig. 3 of the paper) is typical of what we would call today ice-templated silica.

  18. 18.

    The estimated cooling rate is \(10^4~\mathrm{K}\cdot \mathrm{s}^{-1}\), and is thus still lower than the cooling rate required to vitrify water (\(10^6~\mathrm{K}\cdot \mathrm{s}^{-1}\)). Crystalline ice is thus formed.

  19. 19.

    See p. 123.

  20. 20.

    See p. 494.

  21. 21.

    See p. 390 and following.

  22. 22.

    See p. 378.

  23. 23.

    See p. 152.

  24. 24.

    See p. 154.

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Deville, S. (2017). Ice-Templating: Processing Routes, Architectures, and Microstructures. In: Freezing Colloids: Observations, Principles, Control, and Use. Engineering Materials and Processes. Springer, Cham. https://doi.org/10.1007/978-3-319-50515-2_4

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