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Neutron Spectroscopy Study of the Diffusivity of Hydrogen in Mos2

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Neutron Spectroscopy Study of the Diffusivity of Hydrogen in Mos2 PCCP View Article Online PAPER View Journal | View Issue Neutron spectroscopy study of the diffusivity of hydrogen in MoS2 Cite this: Phys. Chem. Chem. Phys., 2021, 23, 7961 Vitalii Kuznetsov, ab Wiebke Lohstroh,c Detlef Rogalla,d Hans-Werner Becker,d Thomas Strunskus,e Alexei Nefedov, f Eva Kovacevic,g Franziska Traegerb and Peter Fouquet *a The diffusion of hydrogen adsorbed inside layered MoS2 crystals has been studied by means of quasi- elastic neutron scattering, neutron spin-echo spectroscopy, nuclear reaction analysis, and X-ray Received 29th September 2020, photoelectron spectroscopy. The neutron time-of-flight and neutron spin-echo measurements Accepted 18th December 2020 demonstrate fast diffusion of hydrogen molecules parallel to the basal planes of the two dimensional DOI: 10.1039/d0cp05136e crystal planes. At room temperature and above, this intra-layer diffusion is of a similar speed to the surface diffusion that has been observed in earlier studies for hydrogen atoms on Pt surfaces. A significantly rsc.li/pccp slower hydrogen diffusion was observed perpendicular to the basal planes using nuclear reaction analysis. Creative Commons Attribution-NonCommercial 3.0 Unported Licence. 1 Introduction in order to replace the expensive platinum, which is widely used today. Diffusion of molecules on surfaces is crucial for a range of Molybdenum disulphide, MoS2, has shown promising beha- chemical processes, such as catalysis or sensing, but it remains viour as a catalyst in the hydrogen evolution reaction (HER),6–10 extremely difficult to observe experimentally on atomic length which is completely in line with its known activity for hydro- scales. This is particularly true for the case of light molecules genation reactions. However, the structural properties are that have few electrons, such as hydrogen. Substantial break- rather complex. MoS2 forms a crystal of hexagonal Mo and S This article is licensed under a throughs in this field have been achieved by quasi-elastic layers, with an interlayer distance of 6.2 Å.11 On the basis of this helium atom scattering (QHAS) and quasi-elastic neutron structure, three stacking variants have been observed, each scattering (QENS) in recent years.1–3 In the following we present with slightly different conductivity and catalytic activity.6,12 a study that exploits QENS in this tradition. In earlier studies catalytic activity had been attributed to Open Access Article. Published on 18 January 2021. Downloaded 9/26/2021 11:40:00 AM. With an increase in renewable energy production, the pro- amorphous particles,13 but recently it has been shown that blem of energy storage becomes more and more significant. although the active centres are probably sulphur edge atoms, One of the most promising ideas is storage in form of hydrogen the stoichiometry of the active surface is 1Mo:2S, the same as gas. It involves the production of hydrogen by electrolysis and for the perfect crystal.6,7,10,14 later reconversion of hydrogen in fuel cells. It is of paramount However, the amount of active centres may not be the only importance for these processes to be carried out most effi- reason for chemical activity. For palladium, for example, during ciently with the most readily accessible materials. Therefore, hydrogen evolution also the movement of hydrogen atoms to there have been intense studies in the search for catalyst sites below the surface has been observed (HIR, hydrogen materials for the hydrogen and oxygen evolution reactions,4,5 injection reaction).15 For platinum surfaces, the recombinative desorption of hydrogen was shown to be the rate limiting step 16 in HER. For MoS2 some theoretical studies suggest that a Institut Laue-Langevin, CS 20156, 38042 Grenoble Cedex 9, France. intercalation of hydrogen is possible. Therefore, the diffusion E-mail: [email protected]; Tel: +33 476 20 7204 b of hydrogen can be expected to play a role in the overall Westfa¨lische Hochschule, Gelsenkirchen, Bocholt, Recklinghausen, 17,18 August-Schmidt-Ring 10, 45665 Recklinghausen, Germany reaction mechanism. c Technische Universita¨tMu¨nchen, Forschungsneutronenquelle Heinz Maier-Leibnitz Within the scope of the present study we investigated the (FRM II), Lichtenbergstr. 1, 85747 Garching, Germany adsorption and diffusion of hydrogen on MoS2 using quasi- d RUBION, Ruhr-Universita¨t Bochum, Universita¨tsstr. 150, 44801 Bochum, Germany elastic neutron scattering (QENS) and neutron spin-echo e Technische Fakulta¨t der Universita¨t Kiel, Institut fu¨r spectroscopy (NSE) together with nuclear reaction analysis Materialwissenschaft-Materialverbunde, Kaiserstr. 2, 24143 Kiel, Germany f Karlsruher Institut fu¨r Technologie (KIT), Institut fu¨r Funktionelle Grenzfla¨chen (NRA) and X-ray photoelectron spectroscopy (XPS). (IFG), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany This paper is organised as follows: after this short introduc- g GREMI, UMR 7344 CNRS/Universite´ d’Orle´ans, 45067 Orle´ans, Cedex 2, France tion, we will give a short description of the theoretical model This journal is © the Owner Societies 2021 Phys. Chem. Chem. Phys., 2021, 23, 7961–7973 | 7961 View Article Online Paper PCCP thatweusetoanalysethespectroscopic neutron scattering data. describing the motion of hydrogen atoms, the rotational terms Then, we will describe the sample preparation and the experimental disappear (SR(Q,o) d(o)). apparatus that we used. Finally we will describe our experimental Depending on a system, translational motion can either findings and discuss them in the framework of earlier studies. have a free or a spatially constrained behaviour. In the former case it can be expressed as a simple normalised Lorentzian 1 GðQÞ 2 Theory STðQ; oÞ¼LðGðQÞ; oÞ¼ . In the latter case a part po2 þ G2ðQÞ A general equation describing the incoherent neutron scatter- of the quasi-elastic scattering remains elastic and a delta- 2 2 ing off the adsorbed hydrogen consists of four parts: the function term, A0(Q)d(o), is added: ÀQ2 u2 Debye–Waller factor, S ðQÞ¼exp , the elastic ST(Q,o)=A0(Q)d(o)+(1À A0(Q))L(GT,o), (3) DW 3 scattering function, Sel(Q,o), the quasi-elastic scattering func- where A0(Q) is called an elastic incoherent structure factor 26 tion, Sqe(Q,o), and a resolution function R(Q,o): (EISF). For confinement within a sphere of radius rc it can be written as:27 S(Q,o)=SDW(Q)d(o)*[Sel(Q)d(o)+(1À Sel(Q))Sqe(Q,o)] 2 * R(Q,o). (1) 3j1 ðÞQrc A0ðQÞ¼ 2 2 : (4) Q rc Q = ki À kf is the momentum transfer and ho = Ef À Ei is the energy transfer of the neutron upon scattering with ki and kf In the following we will use the confined diffusion model since being the initial and final momenta, and Ei and Ef being the hydrogen motion in a layered MoS2 is naturally constrained by initial and final energies of the neutron, respectively. h is the the MoS2 matrix. Sqe can then be expressed as: reduced Planck constant. The symbol * describes a convolution à action. The term, which contains the most important informa- SqeðQ; oÞ¼STðQ; oÞ SRðQ; oÞ Creative Commons Attribution-NonCommercial 3.0 Unported Licence. tion about the diffusive dynamics in the system, is S (Q,o). We qe ¼ ½A ðQÞdðoÞþ½Á1 À A ðQÞ LðÞG ; o will consider a model developed by Sears based on the first 0 0 T "# Born approximation for the case of a moving polyatomic X1 ÀÁ à 2 2 l molecule exhibiting both translational and rotational motion j0 ðQRÞdðoÞþ ð2l þ 1Þjl ðQRÞL GR; o : with negligible correlations between them.19,20 The model l¼1 has been applied successfully to a wide range of molecules (5) in confinement, including hydrogen, water, benzene and neopentane.21–24 For undercooled water the approximation of The convolution in eqn (5) can be performed explicitly, giving: This article is licensed under a negligible correlations was tested by molecular dynamics 2 SqeðQ; oÞ¼A0ðQÞj0 ðQRÞdðoÞ simulations and shown to be applicable at temperatures where 25 X1 ÀÁ molecules are free to move and rotate. For hydrogen molecules 2 l þ A0ðQÞ ð2l þ 1Þjl ðQRÞL GR; o in MoS2, due to the low hydrogen density, the translational– Open Access Article. Published on 18 January 2021. Downloaded 9/26/2021 11:40:00 AM. l¼1 rotational decoupling can be assumed to be valid for diffusion 2 within the layers of MoS2. For the diffusion perpendicular to the þ ½1 À A0ðQÞ j0 ðQRÞLðÞGT; o layers, however, this approximation might be difficult to apply X1 ÀÁ due to the spacial confinement. Since we are mainly interested in 2 l þ ½1 À A0ðQÞ ð2l þ 1Þjl ðQRÞL GT þ GR; o : the hydrogen motion within the layers, however, we consider that l¼1 the approximation of negligible correlations is reasonable. In this (6) case Sqe(Q,o) can be represented by a convolution of transla- tional, ST(Q,o), and rotational, SR(Q,o), components, respectively. A quasi-elastic broadening caused by translational diffusion 19 The rotational component is described by: GT depends heavily on the type of motion, which can be X1 ÀÁ continuous or jump-like. A number of different models have 2 2 l SRðQ; oÞ¼j0 ðQRÞdðoÞþ ð2l þ 1Þjl ðQRÞL GR; o ; (2) been considered that describe each kind of diffusion as usually l¼1 several of them need to be tested on a system in order to get a reliable result. Three models will be discussed in detail later in where j (x) is a spherical Bessel function of the first kind of order l the Results and discussion section. l, d(o) is the Dirac delta function, R is the radius of gyration of a l Here, we will consider a commonly occurring case, GR { GT, 1 G l which allows us to neglect GR in the last series in (6).
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