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Hydrogen Sorption Properties of Materials

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Hydrogen Storage Materials

Part of the book series: Green Energy and Technology ((GREEN))

Abstract

In this chapter we examine the hydrogen sorption properties of materials, considering both the parameters that are of prime practical engineering importance, and the thermodynamic and kinetic properties of interest for future materials development. We begin with the practical storage properties, such as the reversible storage capacity, including definitions of the gravimetric and volumetric capacities and the total and excess adsorption for adsorptive hydrogen storage, the long term cycling stability, gaseous impurity resistance, and the ease of activation. The thermodynamic properties, including the enthalpy of molecular hydrogen adsorption and the enthalpy of hydride formation or decomposition are then covered. We then discuss the kinetics of hydrogen adsorption and absorption, including parameters such as the activation energy, hydrogen diffusion coefficient and the apparent rates of absorption or desorption, which can be used to characterise the time-dependent sorption and desorption properties of materials. The latter part of the chapter then considers both equilibrium and kinetic models that can be used to describe experimental data.

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Notes

  1. 1.

    The natural abundance is significant if a material is to be used in bulk quantities in the automotive industry [1], but less so for niche applications.

  2. 2.

    The materials representing the extreme of this case are the kinetically stabilised hydrides [2].

  3. 3.

    There will always be some discrepancy because isotherms are not typically vertical in the single phase regions (on a pressure against composition plot) and, in addition, some residual hydrogen is usually trapped in the sample after dehydrogenation.

  4. 4.

    The critical H/M ratio is x crit = 0.29 and the critical pressure, P crit = 2.015 MPa [4].

  5. 5.

    The term adsorbed phase is used to describe the hydrogen that can be considered adsorbed and so therefore not in the bulk hydrogen gas phase.

  6. 6.

    The unit recommended in the IUPAC adsorption measurement guidelines is mol g−1 [8].

  7. 7.

    This does not, however, determine the actual volumetric storage capacity of a practical hydrogen store constructed using the material because this will depend on the bulk density of the storage bed (see Sect. 6.2.1).

  8. 8.

    The reverse is also necessary in order to compare theoretical, or simulated, hydrogen adsorption capacities directly with experimental data, although this is less of a concern here because we are interested in the experimental determination of hydrogen adsorption capacity.

  9. 9.

    See Murray et al. [14], a review on hydrogen storage by MOFs, in which the total adsorption is defined as the amount of hydrogen contained within the boundaries formed by the faces of the framework crystals, although this is only the case if the total pore volume approximation is used.

  10. 10.

    The measured SSA depends on the diameter of the adsorbate molecule and the chosen method. In addition, a ‘surface layer’, which does not physically form on the internal surfaces of micropores, would be three dimensional in the smallest pores. A material consisting exclusively of perfect slit-shaped pores would perhaps be an exception, but this is an idealised scenario that is unlikely to occur in practice. See Sect. 5.2.4 for further discussion of the applicability of the concept of surface area for microporous materials.

  11. 11.

    See Fig. 6.2, Sect. 6.6.2, for an example of this correction applied to hydrogen adsorption data for an activated carbon.

  12. 12.

    So-called pipe diffusion.

  13. 13.

    See, for example, the study of the performance of three AB5 compounds by Wanner et al. [27] in which each sample was subjected to approximately 95,000 thermally induced hydrogen absorption/desorption cycles.

  14. 14.

    If a good understanding of the hydrogen sorption properties of a material is to be obtained, its performance using high purity hydrogen should be determined initially before the controlled introduction of impurities. The performance using high purity hydrogen will then act as a baseline measurement against which future comparisons can be made.

  15. 15.

    Further details can be found in Yang [38].

  16. 16.

    The definition of activation in the JIS glossary of terms is ‘a promotion of reaction for absorption and desorption of hydrogen absorbing alloys’ [32].

  17. 17.

    This is also known as the ‘isosteric heat’, although this terminology is less precise and so ‘isosteric enthalpy of adsorption’ is preferable.

  18. 18.

    Zn3(BDC)3[Cu(Pyen)], where H2BDC = 1,4 benzenedicarboxylic acid and PyenH2 = 5-methyl-4-oxo-1,4-dihydro-pyridine-3-carbaldehyde.

  19. 19.

    An increase in the isosteric enthalpy of adsorption can occur due to increased adsorbate–adsorbate interactions [12] but this does not apply to supercritical hydrogen adsorption in microporous materials.

  20. 20.

    This argument is stronger in the case of hydrides partly because there is a larger range of formation enthalpy values for hydrogen absorption compared to the adsorption enthalpies for physisorption, which typically range from −4 to −12 kJ mol−1 (adsorption is always exothermic). In contrast, to use somewhat extreme examples, according to Buschow et al. [71], the enthalpy of hydride formation can range from −225 to +52 kJ mol−1 for the binary hydrides (hydrogen absorption can be both endo- and exothermic). Therefore, a relatively constant ΔS can be ignored when determining whether a given hydride is likely to form at practical temperatures and pressures.

  21. 21.

    Further discussion of this is given by Buschow et al. [71].

  22. 22.

    The kinetically stabilised hydrides mentioned briefly in Sect. 2.2.3 are a possible exception.

  23. 23.

    One example is fully activated Pd0.85Ni0.15 alloy, which exhibits no hysteresis [75].

  24. 24.

    As an example, MgH2 shows practically useful gravimetric and volumetric hydrogen storage capacities but the slow kinetics of hydrogen uptake and release mean that much of the research into MgH2 and Mg-based hydrides for storage purposes has focused on the enhancement of the rates of hydrogen absorption and desorption by these materials; for example, by mechanical milling of the hydride, either to modify the microstructure and particle morphology or to mix the material with an appropriate additive (see Sects. 2.2.3 and Sect. 2.2.4.1).

  25. 25.

    According to Ruthven [76] the terminology can vary in the literature and so this is also known as micropore diffusion, configurational diffusion and intracrystalline diffusion.

  26. 26.

    The formation and growth of the hydride phase is not straightforward and can take many forms. The observation of the initial stages of hydride formation has been performed for some bulk hydride samples [84], but is experimentally challenging. There have also been a large number of surface studies of hydrogen adsorption on nearly perfect single crystal surfaces [86]. However, extrapolation of these results to real samples and elevated hydrogen pressure suffers from what has become known in surface science and catalysis as the materials, complexity and pressure gaps [87, 88]. The first two relate to the difference between near perfect single crystal samples and real (polycrystalline and heterogeneous) materials, and the latter to the difference between the nature of gas–solid interactions in Ultra-High Vacuum (UHV) environments and gas–solid interactions at the elevated pressures encountered in real applications.

  27. 27.

    An alternative view is that the β phase nucleates randomly throughout the bulk of the particle. This tends to be called the nucleation and growth model, although in both cases the hydride phase must initially nucleate and then grow. According to Bloch and Mintz [84], in pure metals, nuclei form initially at the locations of the highest hydrogen concentration and the lowest activation energy for nucleation. These locations will include bulk discontinuities such as grain boundaries and defects. In detailed studies, different groups of nuclei have been observed, each with different relative rates of nucleation and growth, so that some groups rapidly form a large number of nuclei that grow slowly, whereas others slowly form a small number of nuclei that grow rapidly. The growth of the nuclei can also be anisotropic in terms of crystallographic direction. Hydride formation follows the hydrogen concentration gradient in the host metallic lattice. Hydrogen tends to accumulate under the surface passivation layer, the protective oxide coating discussed in Sect. 3.1.4, and so this is where the nucleation begins. If there is rapid hydrogen diffusion through grain boundaries, nucleation can then occur at greater depths. In the case of powder samples, however, for which the surface area-to-volume ratio is large, the surface region is the most likely location for hydride nucleation.

  28. 28.

    Fowler [106] derived the Langmuir equation using essentially the same assumptions that the atoms or molecules are adsorbed on definite adsorption sites, only one adsorbate atom or molecule can be accommodated on each site and that the energy of each is unaffected by the presence of neighbouring adsorbate atoms or molecules.

  29. 29.

    Note that n in this case should be the absolute adsorbed quantity (see Sect. 3.1.1.3).

  30. 30.

    In addition to the assumption of a homogeneous surface, another fundamental assumption in the derivation of the Langmuir equation is that the enthalpy of adsorption does not vary with the amount of gas adsorbed [104]. This has been shown experimentally not to be the case for supercritical hydrogen adsorption on a number of microporous adsorbents, which further supports the inapplicability of the Langmuir equation.

  31. 31.

    Henry’s law describes a linear uptake with pressure at low surface coverage, due to the absence of competition for adsorption sites and the non-interaction of neighbouring adsorbate molecules or atoms. The latter is expected to be the case for very low adsorbate concentrations (see also Sect. 3.2.1).

  32. 32.

    The adsorbed quantity should saturate because it cannot increase indefinitely.

  33. 33.

    According to Do [36], values for a strongly activated carbon are typically between 1.2 and 1.8, and for zeolites between 3 and 6, although Rouquerol et al. [12] quote values between 2 and 6 from original work by Dubinin, and Lowell et al. [105] mention the range 2–5.

  34. 34.

    http://webbook.nist.gov/chemistry/, accessed 13th January 2010.

  35. 35.

    Note that T crit is the temperature of the critical point for the two phase co-existence region of the palladium–hydrogen system, not that of fluid phase hydrogen (see Sect. 3.1.1).

  36. 36.

    In this regard, it is not a materials problem that requires a solution, although it is still of scientific interest.

  37. 37.

    See Johansson et al. [148] for a discussion of the validity of this dependence, as well as comments on the variability of experimental results in Christmann [86].

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    Darren P. Broom

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Broom, D.P. (2011). Hydrogen Sorption Properties of Materials. In: Hydrogen Storage Materials. Green Energy and Technology. Springer, London. https://doi.org/10.1007/978-0-85729-221-6_3

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