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Application Overview There is currently a great deal of interest in the use of solid state materials for the storage of hydrogen, and hence the characterisation of the hydrogen sorption properties of these materials.
There are three main gas sorption techniques that can be used for the evaluation of the hydrogen storage capacities and sorption properties of a material: gravimetric and volumetric isotherm determination, and temperature-programmed desorption (TPD), also known as thermal desorption spectroscopy (TDS). Hiden Isochema offer products that use all three of these techniques, as well as having considerable in-house expertise and experience in the performance of hydrogen sorption measurements.
Hydrogen Storage Products: IGA-001 , IGA-003 , HTP1-V , HTP1-S
IGA-001
The IGA-001 was originally developed specifically for the determination of hydrogen uptake isotherms using the gravimetric method, in order to improve the accuracy of PCT isotherm data compared with conventional methods [1]. The analyser has a UHV vessel construction but can also withstand high pressures and temperatures in order to suit studies of diverse storage media, including rechargeable metal hydrides [1-5], nitrides [6], nanostructured carbons [7-9], metal-organic frameworks (MOFs) [10,11], zeolites [12,13] and microporous polymers [14,15]. It is ideally suited to the measurement of the adsorption of hydrogen on microporous materials that require high vacuum degassing conditions.
The range of applications includes hydrogen storage capacity, automatic isotherm determination at one or more temperatures, real-time kinetic analysis including hydriding (phase transition) analysis, PCI, and the ability to perform surface area analysis, e.g., to assess embrittlement.
The IGA-003 instrument extends this range of applications to enable the measurement of the effects of impurities and it can also perform TPD-MS experiments.
HTP1-V
The HTP1-V is a volumetric instrument offering unrivalled accuracy in the determination of pressure-composition isotherms (PCIs) and excess adsorption isotherms at elevated pressures. The system is controlled through the HTPwin software, which allows the automated measurement of isotherms with control over a number of measurement parameters, and offers unique features such as the measurement of isobaric kinetic data using mass flow controllers (MFCs). Through the integration of the MFC signal, this provides an accurate measurement of the charging and discharging of the material with time, at a fixed pressure, to mimic the performance of the material in a real storage situation.
HTP1-S
The HTP1-S is a thermal desorption analyser that allows the hydrogen desorption spectrum to be determined over a wide temperature range, from very small sample sizes. The HTP1-S also offers volumetric measurement capability that allows an absorption isotherm to be measured before the performance of a thermal desorption spectrum. The thermal desorption spectrum is measured using a mass spectrometer and the signal calibrated through the use of a flow of a calibrant gas mixture. The use of a quadrupole mass spectrometer also allows the user to perform a number of other operations, such as the monitoring of the degassing of samples during the activation process and the identification of possible decomposition products during the dehydrogenation process. The HTP1-S was recently used to obtain TDS data for a nanostructured Mg-H2 material [16].
Selected references featuring data measured using Hiden Isochema hydrogen storage material characterisation products are in the reference list below.
Product Information Pages
IGA-001
IGA-003
HTP1-V
HTP1-S
Application Notes
Article 118 The Characterisation of Gas Storage Media using the IGA System Article 125 The Activation of LaNi5-H Please use our enquiry form to request either of these application notes.
References
[1] Experimental Determination of Sorption-Desorption Isotherms by Computer-Controlled Gravimetric Analysis
M. J. Benham and D. K. Ross
Zeitschrift für Physikalische Chemie NF 163 (1989) S25
[2] The Measurement of Concentration-Dependent Hydrogen Diffusion Coefficients in the Solid-Solution Alloy Pd-Y
P. R. Stonadge, M. J. Benham and D K Ross
Separation Technology, Ed E F Vansant (Elsevier) (1994) 129
[3] Enhanced Hydrogen Sorption Capacities and Kinetics of Mg2Ni Alloys by Ball-milling with Carbon and Pd Coating
R. Janot, L. Aymard, A. Rougier, G.A. Nazri, J.M. Tarascon
Journal of Alloys and Compounds, 356 (2003) 438-441
[4] Hydrogenation Properties of Nanocrystalline Mg- and Mg2Ni-Based Compounds Modified with Platinum Group Metals (PGMs)
O. Gutfleisch, N. Schlorke-de Boer, N. Ismail, M. Herrich, A. Walton, J. Speight, I. R. Harris, A. S. Pratt, A. Züttel
Journal of Alloys and Compounds 356-357 (2003) 598-603
[5] Fast Hydrogen Sorption Kinetics for Ball-Milled Mg2Ni Alloys
R. Janot, L. Aymard, A. Rougier, G. A. Nazri, J. M. Tarascon
Journal of Physics and Chemistry of Solids, 65 (2-3), (2004) 529-534
[6] Interaction of Hydrogen with Metal Nitrides and Imides
P. Chen, Z. Xiong, J. Luo, J. Lin and K. L. Tan
Nature 420 (2002) 302-304
[7] Large Cryogenic Storage of Hydrogen in Carbon Nanotubes at Low Pressures
B. K.Pradhan, A. Harutyunyan, D. Stojkovic, P. Zhang, M. W. Cole, V. Crespi, H. Goto, J. Fujiwara and P. C. Eklund
Journal of Materials Research 17 (2002) 2209-2222
[8] Hydrogen Adsorption on a Single-Walled Carbon Nanotube Material : A Comparative Study of three different Adsorption Techniques
A. Ansón, M. A. Callejas, A. M. Benito, W. K. Maser, M. J. Benham, J. Jagiello, A. Züttel, M. T. Martínez
Nanotechnology 15 (2004) 1503-1508
[9] Hydrogen Adsorption on Functionalized Nanoporous Activated Carbons
X. B. Zhao, B. Xiao, A. J. Fletcher, and K. M. Thomas
Journal of Physical Chemistry B 109 (2005) 8880-8888
[10] Hysteretic Adsorption and Desorption of Hydrogen by Nanoporous Metal Organic Frameworks
X. Zhao, B. Xiao, A. J. Fletcher, K. M. Thomas, D. Bradshaw, M. J. Rosseinsky
Science 306 (2004) 1012-1015
[11] High H2 Adsorption by Coordination-Framework Materials
X. Lin J. Jia, X. Zhao, K. M. Thomas, A. J. Blake, G. S. Walker, N. R. Champness, P. Hubberstey, M. Schröder
Angewandte Chemie International Edition 45 (2006) 7358 - 7364
[12] Hydrogen Adsorption in Zeolites A, X, Y and RHO
H. W. Langmi, A. Walton, M. M. Al-Mamouri, S.R. Johnson, D. Book, J. D. Speight, P. P. Edwards, I.Gameson, P. A. Anderson and I. R. Harris
Journal of Alloys and Compounds 356-357 (2003) 710-715
[13] Hydrogen storage in ion-exchanged zeolites
H. W. Langmi, D. Book, A. Walton, S. R. Johnson, M. M. Al-Mamouri, J. D. Speight, P. P. Edwards, I. R. Harris, P. A. Anderson
Journal of Alloys and Compounds 404-406 (2005) 637-642
[14] Towards polymer-based hydrogen storage materials: engineering ultramicroporous cavities within polymers of intrinsic microporosity
N. B. McKeown, B. Gahnem, K. J. Msayib, P. M. Budd, C. E. Tattershall, K. Mahmood, S. Tan, D. Book, H. W. Langmi, A. Walton
Angewandte Chemie International Edition 45 (2006) 1804-1807
[15] Hydrogen adsorption in microporous hypercrosslinked polymers
J- Y. Lee, C. D. Wood, D. Bradshaw, M. J. Rosseinsky, A. I. Cooper
Chemical Communications 25 (2006) 2670-2672 [16] Hydrogen desorption studies of the Mg24Y5-H system: Formation of Mg tubes, kinetics and cycling effects
C. Zlotea, M. Sahlberg, S. Özbilen, P. Moretto, Y. Andersson
Acta Materialia 56(11) (2008) 2421-2428
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