Structural transformation of layered double hydroxides: an in situ TEM analysis

被引:81
作者
Hobbs, Christopher [1 ,2 ,3 ,4 ]
Jaskaniec, Sonia [2 ,3 ,5 ]
McCarthy, Eoin K. [2 ,3 ,4 ]
Downing, Clive [2 ,3 ,4 ]
Opelt, Konrad [6 ]
Guth, Konrad [6 ]
Shmeliov, Aleksey [1 ,4 ]
Mourad, Maurice C. D. [7 ]
Mandel, Karl [8 ,9 ]
Nicolosi, Valeria [2 ,3 ,5 ]
机构
[1] TCD, Sch Phys, Dublin, Ireland
[2] TCD, AMBER, Dublin, Ireland
[3] TCD, CRANN, Dublin, Ireland
[4] TCD, CRANN, Adv Microscopy Lab, Dublin, Ireland
[5] TCD, Sch Chem, Dublin, Ireland
[6] Fraunhofer Project Grp Mat Recycling & Resource S, D-63457 Hanau, Germany
[7] TNO, Dept Mat Solut, Eindhoven, Netherlands
[8] Fraunhofer Inst Silicate Res ISC, Neunerpl 2, D-97082 Wurzburg, Germany
[9] Julius Maximilians Univ Wurzburg, Dept Chem & Pharm, Chair Chem Technol Mat Synth, Rontgenring 11, D-97070 Wurzburg, Germany
关键词
THERMAL-DECOMPOSITION; HYDROTALCITE; CATALYST; EVOLUTION; RETARDANCY; MORPHOLOGY; CONVERSION; NANOSHEETS; CLAYS; ANION;
D O I
10.1038/s41699-018-0048-4
中图分类号
TB3 [工程材料学];
学科分类号
0805 ; 080502 ;
摘要
A comprehensive nanoscale understanding of layered double hydroxide (LDH) thermal evolution is critical for their current and future applications as catalysts, flame retardants and oxygen evolution performers. In this report, we applied in situ transmission electron microscopy (TEM) to extensively characterise the thermal progressions of nickel-iron containing (Ni-Fe) LDH nanomaterials. The combinative approach of TEM and selected area electron diffraction (SAED) yielded both a morphological and crystallographic understanding of such processes. As the Ni-Fe LDH nanomaterials are heated in situ, an amorphization occurred at 250 degrees C, followed by a transition to a heterogeneous structure of NiO particles embedded throughout a NiFe2O4 matrix at 850 degrees C, confirmed by high-resolution TEM and scanning TEM. Further electron microscopy characterisation methodologies of energy-filtered TEM were utilised to directly observe these mechanistic behaviours in real time, showing an evolution and nucleation to an array of spherical NiO nanoparticles on the platelet surfaces. The versatility of this characterisation approach was verified by the analogous behaviours of Ni-Fe LDH materials heated ex situ as well as parallel in situ TEM and SAED comparisons to that of an akin magnesium-aluminium containing (Mg-Al) LDH structure. The in situ TEM work hereby discussed allows for a state-of-the-art understanding of the Ni-Fe material thermal evolution. This is an important first, which reveals pivotal information, especially when considering LDH applications as catalysts and flame retardants.
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页数:10
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