{"id":{"repo_id":"birmingham","oai_identifier":"oai:etheses.bham.ac.uk:1008"},"canonical_url":"https://search.dev.ndltd.org/etd/birmingham/oai:etheses.bham.ac.uk:1008","repository":{"repo_id":"birmingham","name":"University of Birmingham","base_url":"https://etheses.bham.ac.uk/cgi/oai2"},"display":{"title":"An investigation into the synthesis and characterisation of metal borohydrides for hydrogen storage","abstract":"With relatively high gravimetric and volumetric hydrogen storage capacities, borohydride compounds are being investigated for their potential use as hydrogen storage media. A study has been made into the mechanical milling of metal chlorides with sodium borohydride to try to form homoleptic borohydrides. Mechanical milling of zinc chloride with sodium borohydride resulted in the formation of a covalent complex NaZn\\(_2\\)(BH\\(_4\\))\\(_5\\). Thermal decomposition occurred at 80°C with a mass change of 12 wt.%, associated with the evolution of hydrogen and diborane. A composite mixture with magnesium hydride a reaction between diborane and magnesium hydride was observed form magnesium borohydride. Mechanical milling of calcium chloride or magnesium chloride with sodium borohydride did not produce calcium borohydride and magnesium borohydride, but rather resulted in solid solutions where chlorine ions substitute for borohydride ions within the cubic sodium borohydride lattice. Thermal decomposition of milled calcium chloride and sodium borohydride occurs at a similar manner to that of Ca(BH\\(_4\\))\\(_2\\) (from Sigma-Aldrich). Milled magnesium chloride and sodium borohydride thermally decomposes via several unknown phases with a weight loss of 4.4 wt.% yielding Mg, MgB\\(_2\\), B, and [B\\(_{12}\\)H\\(_{12}\\)]\\(^{2-}\\). Lithium borohydride investigated using Raman spectroscopy. After heating lithium borohydride through its orthorhombic to hexagonal phase change (118°C) and melting point (280°C), shifts in Raman peak position and peak width were measured as a function of temperature. This work shows the in-situ decomposition of LiBH\\(_4\\) observing formation of lithium dodecaborane (Li\\(_2\\)B\\(_{12}\\)H\\(_{12}\\)) at 340°C and amorphous boron from liquid lithium borohydride.","abstract_html":"With relatively high gravimetric and volumetric hydrogen storage capacities, borohydride compounds are being investigated for their potential use as hydrogen storage media. A study has been made into the mechanical milling of metal chlorides with sodium borohydride to try to form homoleptic borohydrides. Mechanical milling of zinc chloride with sodium borohydride resulted in the formation of a covalent complex NaZn<span class=\"etd-inline-math\"><sub>2</sub></span>(BH<span class=\"etd-inline-math\"><sub>4</sub></span>)<span class=\"etd-inline-math\"><sub>5</sub></span>. Thermal decomposition occurred at 80°C with a mass change of 12 wt.%, associated with the evolution of hydrogen and diborane. A composite mixture with magnesium hydride a reaction between diborane and magnesium hydride was observed form magnesium borohydride. Mechanical milling of calcium chloride or magnesium chloride with sodium borohydride did not produce calcium borohydride and magnesium borohydride, but rather resulted in solid solutions where chlorine ions substitute for borohydride ions within the cubic sodium borohydride lattice. Thermal decomposition of milled calcium chloride and sodium borohydride occurs at a similar manner to that of Ca(BH<span class=\"etd-inline-math\"><sub>4</sub></span>)<span class=\"etd-inline-math\"><sub>2</sub></span> (from Sigma-Aldrich). Milled magnesium chloride and sodium borohydride thermally decomposes via several unknown phases with a weight loss of 4.4 wt.% yielding Mg, MgB<span class=\"etd-inline-math\"><sub>2</sub></span>, B, and [B<span class=\"etd-inline-math\"><sub>12</sub></span>H<span class=\"etd-inline-math\"><sub>12</sub></span>]<span class=\"etd-inline-math\"><sup>2-</sup></span>. Lithium borohydride investigated using Raman spectroscopy. After heating lithium borohydride through its orthorhombic to hexagonal phase change (118°C) and melting point (280°C), shifts in Raman peak position and peak width were measured as a function of temperature. This work shows the in-situ decomposition of LiBH<span class=\"etd-inline-math\"><sub>4</sub></span> observing formation of lithium dodecaborane (Li<span class=\"etd-inline-math\"><sub>2</sub></span>B<span class=\"etd-inline-math\"><sub>12</sub></span>H<span class=\"etd-inline-math\"><sub>12</sub></span>) at 340°C and amorphous boron from liquid lithium borohydride.","abstract_has_math":true,"creators":["Reed, Daniel Thomas"],"institution":"University of Birmingham","degree_name":"d_ph","degree_level":"d_ph","degree_discipline":null,"degree_department":null,"school":null,"contributors":[],"advisors":[],"committee_chairs":[],"committee_members":[],"year":2010,"date_issued":"2010-07","date_published":"2010-07","updated_at":"2026-07-24T01:11:19Z","subjects":["TJ Mechanical engineering and machinery","TP Chemical technology","TN Mining engineering. Metallurgy"],"languages":[],"rights":[],"rights_urls":[],"identifier_entries":[]},"links":{"outbound_url":null,"outbound_label":null,"outbound_source":null},"metadata_groups":[{"id":"people","label":"People","entries":[{"key":"dc:contributor.sponsor","label":"Sponsor","values":["epsrc"]},{"key":"dc:creator","label":"Author","values":["Reed, Daniel Thomas"]}]},{"id":"academic_context","label":"Academic Context","entries":[{"key":"dc:date","label":"Dc Date","values":["2010-07"]},{"key":"dc:date.issued","label":"Date","values":["2010-07"]},{"key":"dc:publisher.department","label":"Dc Publisher Department","values":["College of Engineering & Physical Sciences","School of Metallurgy and Materials"]},{"key":"dc:publisher.institution","label":"Dc Publisher Institution","values":["University of Birmingham"]},{"key":"dc:relation.isreferencedby","label":"Dc Relation Isreferencedby","values":["http://etheses.bham.ac.uk//id/eprint/1008/"]},{"key":"dc:type","label":"Dc Type","values":["Thesis"]},{"key":"dc:type.qualificationlevel","label":"Dc Type Qualificationlevel","values":["d_ph"]},{"key":"dc:type.qualificationname","label":"Dc Type Qualificationname","values":["d_ph"]}]},{"id":"subjects_keywords","label":"Subjects and Keywords","entries":[{"key":"dc:subject","label":"Dc Subject","values":["TJ Mechanical engineering and machinery","TP Chemical technology","TN Mining engineering. Metallurgy"]}]},{"id":"identifiers","label":"Identifiers","entries":[{"key":"dc:identifier.uri","label":"Identifier URI","values":["http://etheses.bham.ac.uk//id/eprint/1008/1/Reed10PhD.pdf","http://etheses.bham.ac.uk//id/eprint/1008/2/Decl_IS_Reed10PhD.pdf"]}]},{"id":"additional","label":"Additional Metadata","entries":[{"key":"dc:description.abstract","label":"Abstract","values":["With relatively high gravimetric and volumetric hydrogen storage capacities, borohydride compounds are being investigated for their potential use as hydrogen storage media. A study has been made into the mechanical milling of metal chlorides with sodium borohydride to try to form homoleptic borohydrides. Mechanical milling of zinc chloride with sodium borohydride resulted in the formation of a covalent complex NaZn\\(_2\\)(BH\\(_4\\))\\(_5\\). Thermal decomposition occurred at 80°C with a mass change of 12 wt.%, associated with the evolution of hydrogen and diborane. A composite mixture with magnesium hydride a reaction between diborane and magnesium hydride was observed form magnesium borohydride. Mechanical milling of calcium chloride or magnesium chloride with sodium borohydride did not produce calcium borohydride and magnesium borohydride, but rather resulted in solid solutions where chlorine ions substitute for borohydride ions within the cubic sodium borohydride lattice. Thermal decomposition of milled calcium chloride and sodium borohydride occurs at a similar manner to that of Ca(BH\\(_4\\))\\(_2\\) (from Sigma-Aldrich). Milled magnesium chloride and sodium borohydride thermally decomposes via several unknown phases with a weight loss of 4.4 wt.% yielding Mg, MgB\\(_2\\), B, and [B\\(_{12}\\)H\\(_{12}\\)]\\(^{2-}\\). Lithium borohydride investigated using Raman spectroscopy. After heating lithium borohydride through its orthorhombic to hexagonal phase change (118°C) and melting point (280°C), shifts in Raman peak position and peak width were measured as a function of temperature. This work shows the in-situ decomposition of LiBH\\(_4\\) observing formation of lithium dodecaborane (Li\\(_2\\)B\\(_{12}\\)H\\(_{12}\\)) at 340°C and amorphous boron from liquid lithium borohydride."]},{"key":"dc:format","label":"Dc Format","values":["application/pdf"]},{"key":"dc:title","label":"Title","values":["An investigation into the synthesis and characterisation of metal borohydrides for hydrogen storage"]}]}],"canonical_facts":{"dc:contributor.sponsor":["epsrc"],"dc:creator":["Reed, Daniel Thomas"],"dc:date":["2010-07"],"dc:date.issued":["2010-07"],"dc:description.abstract":["With relatively high gravimetric and volumetric hydrogen storage capacities, borohydride compounds are being investigated for their potential use as hydrogen storage media. A study has been made into the mechanical milling of metal chlorides with sodium borohydride to try to form homoleptic borohydrides. Mechanical milling of zinc chloride with sodium borohydride resulted in the formation of a covalent complex NaZn\\(_2\\)(BH\\(_4\\))\\(_5\\). Thermal decomposition occurred at 80°C with a mass change of 12 wt.%, associated with the evolution of hydrogen and diborane. A composite mixture with magnesium hydride a reaction between diborane and magnesium hydride was observed form magnesium borohydride. Mechanical milling of calcium chloride or magnesium chloride with sodium borohydride did not produce calcium borohydride and magnesium borohydride, but rather resulted in solid solutions where chlorine ions substitute for borohydride ions within the cubic sodium borohydride lattice. Thermal decomposition of milled calcium chloride and sodium borohydride occurs at a similar manner to that of Ca(BH\\(_4\\))\\(_2\\) (from Sigma-Aldrich). Milled magnesium chloride and sodium borohydride thermally decomposes via several unknown phases with a weight loss of 4.4 wt.% yielding Mg, MgB\\(_2\\), B, and [B\\(_{12}\\)H\\(_{12}\\)]\\(^{2-}\\). Lithium borohydride investigated using Raman spectroscopy. After heating lithium borohydride through its orthorhombic to hexagonal phase change (118°C) and melting point (280°C), shifts in Raman peak position and peak width were measured as a function of temperature. This work shows the in-situ decomposition of LiBH\\(_4\\) observing formation of lithium dodecaborane (Li\\(_2\\)B\\(_{12}\\)H\\(_{12}\\)) at 340°C and amorphous boron from liquid lithium borohydride."],"dc:format":["application/pdf"],"dc:identifier.uri":["http://etheses.bham.ac.uk//id/eprint/1008/1/Reed10PhD.pdf","http://etheses.bham.ac.uk//id/eprint/1008/2/Decl_IS_Reed10PhD.pdf"],"dc:publisher.department":["College of Engineering & Physical Sciences","School of Metallurgy and Materials"],"dc:publisher.institution":["University of Birmingham"],"dc:relation.isreferencedby":["http://etheses.bham.ac.uk//id/eprint/1008/"],"dc:subject":["TJ Mechanical engineering and machinery","TP Chemical technology","TN Mining engineering. Metallurgy"],"dc:title":["An investigation into the synthesis and characterisation of metal borohydrides for hydrogen storage"],"dc:type":["Thesis"],"dc:type.qualificationlevel":["d_ph"],"dc:type.qualificationname":["d_ph"]},"updated_at":"2026-07-24T01:11:19Z"}