Optically transparent, free‐standing single crystals of the high‐temperature superconductor Bi2Sr2CaCu2O8have been prepared with a typical size ofa×b×c=1 mm×1 mm×1500 A˚. The thickness of the samples has been determined by x‐ray transmission measurements and was found to be uniform to within a lattice spacing. Transmission electron microscopy and diffraction revealed a pseudotetragonal lattice with a twinning free, incommensurate superstructure. X‐ray microanalysis shows that the composition of the sample is homogeneous. Electrical resistivity and magnetic susceptibility measurements indicate that the crystals are good quality superconductors.