2014
DOI: 10.1002/chin.201408230
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ChemInform Abstract: Observation of TiH5 and TiH7 in Bulk‐Phase TiH3 Gels for Kubas‐Type Hydrogen Storage.

Abstract: Storage. -Porous Ti III hydride gels of type (II) are prepared as promising new hydrogen storage materials exploiting the first example of a solid state homoleptic metal hydride that binds further H2 ligands via the Kubas interaction [→ (III)]. These materials use bridging hydride ligands as an ultralight weight structural feature to support a microporous network of Ti binding sites for molecular H 2 chemisorption. High-pressure Raman spectroscopy confirmed the first evidence of TiH5 and TiH7 species. The mate… Show more

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Cited by 2 publications
(5 citation statements)
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“…Although both V(III) and V(IV) are confirmed by XPS and expected to bind H 2 , on the basis of pure VH 4 , 1 H 2 per V gives an expected gravimetric capacity of 3.6 wt % and 2 H 2 per V would amount to 7.3 wt %. Therefore, on the basis of the 5.8 wt % plateau, it is reasonable to assume that some V centers bind 1 H 2 and some bind 2 H 2 , similar to what we have determined for previous Ti, 9 Cr, 10 and V 11 materials. Because the 2.2 m 2 /g surface area of V(IV)-25C−H 2 is very low relative to AX-21, which has a surface area of 2800 m 2 /g and much lower adsorption than V(IV)-25C−H 2 , 27 the hydrogen adsorption of 5.8 wt % cannot be due to physisorption but most likely from the Kubas interaction of H 2 , as directly observed previously by high-pressure Raman spectroscopy for H 2 adsorption by TiH 3 , 9 CrH 3 , 10 and VH 3 .…”
Section: ■ Results and Discussionsupporting
confidence: 80%
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“…Although both V(III) and V(IV) are confirmed by XPS and expected to bind H 2 , on the basis of pure VH 4 , 1 H 2 per V gives an expected gravimetric capacity of 3.6 wt % and 2 H 2 per V would amount to 7.3 wt %. Therefore, on the basis of the 5.8 wt % plateau, it is reasonable to assume that some V centers bind 1 H 2 and some bind 2 H 2 , similar to what we have determined for previous Ti, 9 Cr, 10 and V 11 materials. Because the 2.2 m 2 /g surface area of V(IV)-25C−H 2 is very low relative to AX-21, which has a surface area of 2800 m 2 /g and much lower adsorption than V(IV)-25C−H 2 , 27 the hydrogen adsorption of 5.8 wt % cannot be due to physisorption but most likely from the Kubas interaction of H 2 , as directly observed previously by high-pressure Raman spectroscopy for H 2 adsorption by TiH 3 , 9 CrH 3 , 10 and VH 3 .…”
Section: ■ Results and Discussionsupporting
confidence: 80%
“…Apart from a low angle reflection, suggestive of some mesoscopic order and some small reflections from 25−35°that correspond to the glass capillaries, the majority of the diffraction range does not give rise to reflections establishing that the sample is largely amorphous. This is not surprising as the Ti, 9 Cr, 10 previously synthesized V 11 hydride analogues are also amorphous, and the vanadium region of the XPS discussed below indicates that multiple vanadium species in different oxidation states are present in the material. Thermogravimetric analysis (TGA) was carried out on V(IV)-100 and V(IV)-25C−H 2 to determine the percentage of hydrocarbon remaining in each material after thermal precipitation and subsequent hydrgoeneolysis.…”
Section: ■ Results and Discussionmentioning
confidence: 82%
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“…Similar behavior was already seen in a number of other undercoordinated transition metal centers capable of adsorbing multiple hydrogen molecules in a side-on manner. 10,16,17 In order to elucidate the nature of the surface copper complex before and after hydrogen adsorption, we conducted X-ray photoelectron spectroscopy (XPS) experiments on Cu(OAc) 2 /ACS•H 2 O (Figures 3). As can be seen in Figure 3, the nanocomposite before and after room temperature hydrogen adsorption exhibits Cu 2p XPS features.…”
Section: Resultsmentioning
confidence: 99%
“…The application of eq 2 was for the sake of consistency with previous reports on Kubas compounds prepared by Antonelli's group. 10 Fitted data from eq 2 were used to calculate the isosteric heat of adsorption according to modified Clausius− Clapeyron equation:…”
Section: Experimental Methodsmentioning
confidence: 99%