We report a detailed study of the microstructure and defects in sintered po
lycrystalline magnesium diboride (MgB2). Both transmission electron microsc
opy and X-ray data reveal that MgO is the major second-phase in our bulk sa
mples. Although MgB2 and MgO have different crystal symmetries, being P6/mm
m and Fm-3m, respectively, their stacking sequence of Mg and B (or O) and l
attice spacings in certain crystallographic orientations are very similar.
The size of MgO varies from 10-500 nm, and its mismatch with the MgB2 matri
x can be a source for dislocations. Dislocations in MgB2 often have a Burge
rs vector of < 100 >. 1/3 <1-10 > and 1/3 < 210 > partial dislocations and
their associated stacking faults were also observed. Since both dislocation
s and stacking faults are located in the (001) basal plane, flux pinning an
isotropy is expected. Diffuse scattering analysis suggests that the correla
tion length along the c-axis for defect-free basal planes is about 50 nm. (
001) twist grain boundaries (GBs), formed by rotations along the c-axis, ar
e major grain boundaries in MgB2 as a result of the out-of-plane weak bondi
ng between Mg and B atoms. An excess of Mg was observed in some grain bound
aries. High-resolution nano-probe electron-energy loss spectroscopy reveals
that there is a difference in near edge structure of the boron K-edge acqu
ired from GBs and grain interiors. The change at the edge threshold may be
suggestive of variation of the hole concentration that would significantly
alter boundary superconductivity. (C) 2001 Elsevier Science B.V. All rights
reserved.