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Reciprocal space mapping (RSM) of the relaxor ferroelectric 0.91Pb(Zn1/3Nb2/3)O3-0.09PbTiO3 (PZN-9%PT) single crystals has been performed by using high-resolution synchrotron x-ray diffraction as a function of temperature. The PZN–9%PT crystal consists of tetragonal micro/nanotwin domains and undergoes a sequence of rhombohedral+tetragonal→tetragonal→cubic phase transformation upon heating. The rhombohedral-to-tetragonal temperature occurs at ≅70 °C. The observed RSM patterns can be explained by the micro/nanotwin structures and their corresponding diffraction patterns. [ABSTRACT FROM AUTHOR]