layers. This stacked structure and the order in which the materials are layered are critical in ensuring optimal device performance. A common arrangement of the organic layers within a device is to have a central emissive layer with adjacent charge transport layers. The charge transport layers serve to transport holes or electrons from the electrodes within the device, ideally trapping them in the emissive layer for exciton formation and radiative decay. As such, it is important that the nature and ordering of these layers do not undergo any significant change during device operation as this will lead to a change in performance and in particular the efficiency of the device. It has been observed that exposure to temperatures above ambient (thermal stress) can lead to a significant drop in device performance. [3] It has been suggested that the drop in device performance caused by thermal stress is due to one or more of the organic layers within a device undergoing a glass transition and subsequent accelerated diffusion. [4,5] It is therefore important that the origin of this change in performance is understood, with a specific focus on temperatures that an OLED might be exposed to in a commercial device, either externally, or by joule heating during operation. [6,7] Atomic force microscopy, [8,9] scanning tunneling microscopy, [10] infrared imaging, and impedance spectroscopy [11] have all been used to study the change in film structure on heating. Reflectometry techniques can also be utilized to nondestructively probe the internal layered structure of a multilayer film under thermal stress. For example, studies using X-ray reflectometry showed that a multilayer device containing a copper phthalocyanine (CuPc) hole injection layer, an N,N′-bis(naphthalen-1-yl)-N,N′-diphenylbenzidine (NPB) hole transport layer, a tris(8-hydroxyquinoline)aluminium (Alq 3 ) emissive layer, and a lithium fluoride (LiF) electron injection layer deposited onto ITO on glass maintained discrete layers up to 100 °C, while annealing at 120 °C caused intermixing of the NPB and Alq 3 and the Alq 3 and LiF layers. [12,13] While the electron density differences of the compounds in that particular layered film were sufficient to provide adequate scattering length density (SLD) contrast for the use of X-ray reflectometry, this is generally not the case, particularly for films that primarily comprise A common feature of organic light-emitting diodes is their stacked multilayer structure, which is critical for efficient charge injection and transport, and light emission. In this study, it is found that a blended layer of the holetransport material tris(4-carbazol-9-ylphenyl)amine with 6 wt% fac-tris(2-phenylpyridyl)iridium(III) [Ir(ppy) 3 ] readily undergoes interdiffusion with adjacent layers of typical charge transport materials: bathocuproine; 1,3,5-tris(Nphenylbenzimidazol-2-yl)benzene; N,N′-bis(3-methylphenyl)-N,N′-diphenylbenzidine; and N,N′-bis(naphthalen-1-yl)-N,N′-diphenylbenzidine. This process is followed using combined neutron reflectom...