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A study was conducted on defect structures,orientation relationships, and compositional p r o f i l e s a t DIGMboundaries i n NiXu diffusion couples. TEM revealed dislocations a t the i n i t i a l grain boundary positions of the DIGM zones i n the N i substrate. The misorientation between the DIGM zones and the m t r i x (across the dislocation wall) was determined by electron diffraction and found t o be l e s s than 0.5'. Cu p r o f i l e s across the DIGM zones were obtained by TEMIEDS analysis. The f o m t i o n of the dislocation wall i s discussed i n terms of the misorientation and l a t t i c e misfit between the DIGM zones end the m t r i x .