In this paper we describe the use of combinatorial vapor deposition techniques for the optimization of blue organic light emitting diodes (OLEDs). In these devices the star shaped molecule 1 with a triphenylamine core and three fluorene side groups serves as hole transport and emitting layer. Compound 2 with a much lower lying HOMO and a larger bandgap is used as hole blocking layer. Using combinatorial vapor deposition 42 OLEDs with thickness gradients of both the hole transport and the hole blocking layer have been simultaneously prepared on one substrate. The physical characterization of the devices clearly shows that a hole blocking layer of the star shaped molecule 2 is necessary in order to obtain pure blue emission with CIE coordinates of x = 0.15 and y = 0.15. A thickness of only 5 nm of the blocking layer is sufficient, and with increasing layer thickness the brightness of the blue devices drops. The blue devices exhibit a brightness of 400 cd m–2 and a luminous efficiency of 2 cd A–1. The thickness variations of both the hole transport and the hole blocking layer have been made in one combinatorial evaporation experiment on a single substrate using a set of movable masks. This demonstrates how efficient combinatorial methods can be used for the development of OLEDs.
In this article we present a setup for the combinatorial vapor deposition of thin-film multilayer devices as well as methods for the fast and efficient analytic screening of the libraries obtained. The preparation setup is based on a commercially available evaporation chamber equipped with various evaporation sources for both organic and metallic materials. The combinatorial approach is realized by the combination of a rotation stage for the substrate, a five-mask sampler, and an additional mask whose position can be deliberately varied along one axis during the evaporation process. The latter is used to evaporate linear as well as step gradients by continuous or stepwise movement of a shutter mask. The mask sampler allows to define the sectors of the library and to evaporate more complex structures, e.g., an electrode layout. Finally, the simultaneous evaporation of two or more materials enables us to produce layers of varying composition ratio in general and doped materials, in particular. For the control of the evaporation process we have developed an automation software, which is particularly helpful for complex library designs and which grants excellent repeatability of experiments. Efficient and fast characterization of the obtained libraries is realized by (i) a purely optical setup and (ii) an electro-optical setup. (i) The UV/vis reader FLASHScan 530 permits to map out the UV/vis absorbance or fluorescence of the whole library. The UV/vis absorbance is primarily used to determine layer thicknesses and to confirm thickness uniformity across larger regions. The fluorescence measurements are used to determine the composition of layers containing fluorescent dyes. (ii) For a detailed short- and long-term electro-optical analysis we have developed an automated measurement system, which allows the characterization of 8x8 optoelectronic devices and to study their degradation behavior. Both solar cells and organic light-emitting diodes can be tested. Finally, we have developed a data analysis software to extract characteristic values from the huge amount of data and with this facilitate the finding of systematic dependencies.
Summary: A combinatorial study on the synthesis and in situ orientation of polyimide thin films by vapor deposition polymerization was carried out. The combinatorial libraries consisted of sectors with different thicknesses, compositions, and with or without alignment layers. Monomers were selected to prepare rigid rodlike polyimides and to optimize their orientation during deposition and the imidization process. Vapor deposition of the monomers was performed sequentially or by coevaporation. By using this combinatorial approach the polymerization and the orientation behavior can be simultaneously studied and optimized by variation of film thickness, film composition, and deposition sequence.The combinatorial substrate for sequential evaporation consists of sectors with three PTFE alignment layers (rows B, C, and E) on quartz glass for UV/Vis measurements.magnified imageThe combinatorial substrate for sequential evaporation consists of sectors with three PTFE alignment layers (rows B, C, and E) on quartz glass for UV/Vis measurements.
A combinatorial study on the synthesis and in situ orientation of thin films of aromatic polyimides on different aligning surfaces was carried out. Monomer and polyimide libraries prepared by using a combinatorial approach consisting of step gradients with different thicknesses, sectors with different compositions, and sectors with or without alignment layers were investigated. As aligning surfaces, friction deposited layers of PTFE, rubbed polyimide films, and highly oriented polyimide layers prepared by a shearing technique were used. In addition to 3,39,4,49-biphenyldianhydride (BPDA), only para-linked dianhydrides and diamines with different aspect ratios were utilized.Vapor deposition was performed first with individual monomers, then sequentially or by coevaporation of two or more monomers. By using this combinatorial approach, the monomer and polyimide orientation can be optimized by variation of monomer composition, film thickness, and deposition sequence. The resulting films were characterized regarding their thickness and the achieved degree of orientation by polarized FTIR and UV-vis spectroscopy. The highest degree of orientation indicated by a dichroic ratio of nine to ten was observed for 4,40-diamino-p-terphenyl on PTFE surfaces. For other monomers, dichroic ratios of around two were determined irrespective of the aligning surface, indicating low orientation. It was found that coevaporation of both monomers yields isotropic polyimide films in good quality, whereas sequential evaporation of monomer pairs yields polyimide films with anisotropic properties.
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