PACS 61.14. Lj, 61.66.Bi Higher-Order Laue Zone (HOLZ) rings and their appearance in Electron Backscattered Diffraction (EBSD) pattern from molybdenum were fundamentally investigated in the Scanning Electron Microscope. HOLZ rings of the type 100 , 110 , 111 , 113 and 133 could be unambiguous detected in EBSD pattern of different pure Mo crystals. The [100] HOLZ ring was observed more in detail in dependence on the accelerating energy in the pattern center, and the lattice spacing was determined for all energies. A relatively good accuracy could be obtained for Mo as model sample for problematical high atomic number materials.1 Introduction Electron Backscattered Diffraction (EBSD) is a method to determine crystallographic parameter in the micro and nano range of bulk specimens in the Scanning Electron Microscope (SEM). The main applications are the automatic mapping of the crystal orientation of polycrystalline specimens with known crystal structures, an overview is given e.g. in Ref. [1,2], and the study of interfaces, especially grain boundaries [3,4]. It is also possible to distinguish between different previously selected crystallographic phases, see for example [5,6]. A further advantage is the high lateral resolution of up to 6 nm, which, in this case, could be achieved for a thin platinum film deposited on silicon [7].However, the accuracy in the lattice parameter determination obtained by measuring the width of Kikuchi bands is generally very low and at best only about 5% in dependence on the Kikuchi reflections used, sometimes only 10% [8]. Here, an improvement can allow the exploitation of the so-called HigherOrder Laue Zone (HOLZ) rings. The great advantage of the HOLZ rings are the sharp edges and that their diameter is sensitively dependent on the interplanar spacing perpendicular to the zone axis belonging to it. Conventionally, these HOLZ rings were observed in Kossel-Möllenstedt patterns at convergent beam electron diffraction (CBED) [9] in the Transmission Electron Microscopy (TEM). In some cases HOLZ rings can be observed also in EBSD patterns, but they are not as high in contrast as those in the TEM. HOLZ rings in EBSD patterns have not been sufficiently investigated so far. Baba-Kishi suggested to use HOLZ rings for the measurement of lattice constants, and he recorded a First-Order Laue Zone (FOLZ) ring on film from a marcasite crystal (FeS 2 , orthorhombic) [8]. In Ref.[10] it was shown on GaN thin films that HOLZ rings become more clearly visible by cooling the samples. There is only one paper by Michael and Eades [11] which deals with an evaluation of HOLZ rings. In this contribution, reciprocal lattice layer spacings were measured by means of observed HOLZ rings from different crystal systems using a CCD-based camera system. For compounds with a lower average ordinal number in some cases a good agreement between measured and calculated interplanar crystal spacings could be obtained. However, for higher atomic number materials like Mo, Ta and W the difference between measured and calc...