We report a successful ligand- and liquid-free solid state route to form metal pyrophosphates within a layered graphitic carbon matrix through a single step approach involving pyrolysis of previously synthesized organometallic derivatives of a cyclotriphosphazene. In this case, we show how single crystal Mn2P2O7 can be formed on either the micro- or the nanoscale in the complete absence of solvents or solutions by an efficient combustion process using rationally designed macromolecular trimer precursors, and present evidence and a mechanism for layered graphite host formation. Using in situ Raman spectroscopy, infrared spectroscopy, X-ray diffraction, high resolution electron microscopy, thermogravimetric and differential scanning calorimetric analysis, and near-edge X-ray absorption fine structure examination, we monitor the formation process of a layered, graphitic carbon in the matrix. The identification of thermally and electrically conductive graphitic carbon host formation is important for the further development of this general ligand-free synthetic approach for inorganic nanocrystal growth in the solid state, and can be extended to form a range of transition metals pyrophosphates. For important energy storage applications, the method gives the ability to form oxide and (pyro)phosphates within a conductive, intercalation possible, graphitic carbon as host-guest composites directly on substrates for high rate Li-ion battery and emerging alternative positive electrode materials.
%0 Journal Article
%1 RN89
%A Diaz, C.
%A Valenzuela, M.L.
%A Lavayen, V.
%A O'dwyer, C.
%D 2012
%J Inorganic Chemistry
%K characterization, dqcauchile nanocomposites, nanoparticles, nanotubes, nanowires precursor, pyrolysis, spectroscopic
%N 11
%P 6228-6236
%R 10.1021/ic300767h
%T Layered Graphitic Carbon Host Formation During Liquid-Free Solid State Growth of Metal Pyrophosphates
%U /brokenurl#<Go to ISI>://WOS:000304728500029
%V 51
%X We report a successful ligand- and liquid-free solid state route to form metal pyrophosphates within a layered graphitic carbon matrix through a single step approach involving pyrolysis of previously synthesized organometallic derivatives of a cyclotriphosphazene. In this case, we show how single crystal Mn2P2O7 can be formed on either the micro- or the nanoscale in the complete absence of solvents or solutions by an efficient combustion process using rationally designed macromolecular trimer precursors, and present evidence and a mechanism for layered graphite host formation. Using in situ Raman spectroscopy, infrared spectroscopy, X-ray diffraction, high resolution electron microscopy, thermogravimetric and differential scanning calorimetric analysis, and near-edge X-ray absorption fine structure examination, we monitor the formation process of a layered, graphitic carbon in the matrix. The identification of thermally and electrically conductive graphitic carbon host formation is important for the further development of this general ligand-free synthetic approach for inorganic nanocrystal growth in the solid state, and can be extended to form a range of transition metals pyrophosphates. For important energy storage applications, the method gives the ability to form oxide and (pyro)phosphates within a conductive, intercalation possible, graphitic carbon as host-guest composites directly on substrates for high rate Li-ion battery and emerging alternative positive electrode materials.
@article{RN89,
abstract = {We report a successful ligand- and liquid-free solid state route to form metal pyrophosphates within a layered graphitic carbon matrix through a single step approach involving pyrolysis of previously synthesized organometallic derivatives of a cyclotriphosphazene. In this case, we show how single crystal Mn2P2O7 can be formed on either the micro- or the nanoscale in the complete absence of solvents or solutions by an efficient combustion process using rationally designed macromolecular trimer precursors, and present evidence and a mechanism for layered graphite host formation. Using in situ Raman spectroscopy, infrared spectroscopy, X-ray diffraction, high resolution electron microscopy, thermogravimetric and differential scanning calorimetric analysis, and near-edge X-ray absorption fine structure examination, we monitor the formation process of a layered, graphitic carbon in the matrix. The identification of thermally and electrically conductive graphitic carbon host formation is important for the further development of this general ligand-free synthetic approach for inorganic nanocrystal growth in the solid state, and can be extended to form a range of transition metals pyrophosphates. For important energy storage applications, the method gives the ability to form oxide and (pyro)phosphates within a conductive, intercalation possible, graphitic carbon as host-guest composites directly on substrates for high rate Li-ion battery and emerging alternative positive electrode materials.},
added-at = {2019-12-04T03:57:35.000+0100},
author = {Diaz, C. and Valenzuela, M.L. and Lavayen, V. and O'dwyer, C.},
biburl = {https://www.bibsonomy.org/bibtex/2cdf8658b065f95ae56fc8c2f3c6b313e/dqcauchile},
doi = {10.1021/ic300767h},
interhash = {6a47c1aa4505ccd02a9aff70cf7d3b61},
intrahash = {cdf8658b065f95ae56fc8c2f3c6b313e},
issn = {0020-1669},
journal = {Inorganic Chemistry},
keywords = {characterization, dqcauchile nanocomposites, nanoparticles, nanotubes, nanowires precursor, pyrolysis, spectroscopic},
number = 11,
pages = {6228-6236},
timestamp = {2019-12-04T03:58:17.000+0100},
title = {Layered Graphitic Carbon Host Formation During Liquid-Free Solid State Growth of Metal Pyrophosphates},
type = {Journal Article},
url = {/brokenurl#<Go to ISI>://WOS:000304728500029},
volume = 51,
year = 2012
}