The structure and morphology of the three-dimensional aggregates of ar
achidic acid were studied by atomic force microscopy(AFM) after transf
er onto a silicon wafer and by synchrotron grazing incidence X-ray dif
fraction (GID) at the helium/water interface. The 3D aggregates on the
wafer observed by AFM are islands of granulelike and platelike shapes
. The plate islands consist of terraces of different heights. The crys
tal structure of the plate islands was determined through molecular re
solution by AFM. They have the C-crystal structure of arachidic acid a
t the beginning of the relaxation. During further relaxation the B-cry
stal structure becomes apparent. The islands with B-crystal structure
dominate at the end of the relaxation process. Regions with a disorder
ed molecular structure are found beside the ordered crystal structures
. In all ordered regions of a single island the same crystal structure
is observed. Using GID, the B- and C-crystal structures of the 3D agg
regates of arachidic acid were also found at the helium/water interfac
e. No peaks of any crystal structure are observed until 20% of the mon
olayer material is transformed into 3D aggregates. Then first the peak
s of the B-crystal structure appear, which increase with the relaxatio
n time. Additionally small peaks corresponding to the C-crystal struct
ure are found.