Blichfeld Anders Bank, Bakken Kristine, Chernyshov Dmitry, Glaum Julia, Grande Tor, Einarsrud Mari Ann
Department of Materials Science and Engineering, NTNU Norwegian University of Science and Technology, Sem Saelands vei 12, Trondheim 7491, Norway.
Swiss-Norwegian Beamlines, European Synchrotron Radiation Facility, 71 avenue des Martyrs, Grenoble 38043, France.
J Synchrotron Radiat. 2020 Sep 1;27(Pt 5):1209-1217. doi: 10.1107/S1600577520010140. Epub 2020 Aug 21.
Understanding the crystallization process for chemical solution deposition (CSD) processed thin films is key in designing the fabrication strategy for obtaining high-quality devices. Here, an in situ sample environment is presented for studying the crystallization of CSD processed thin films under typical processing parameters using near-grazing-incidence synchrotron X-ray diffraction. Typically, the pyrolysis is performed in a rapid thermal processing (RTP) unit, where high heating rates, high temperatures and atmosphere control are the main control parameters. The presented in situ setup can reach heating rates of 20°C s and sample surface temperatures of 1000°C, comparable with commercial RTP units. Three examples for lead-free ferroelectric thin films are presented to show the potential of the new experimental set-up: high temperature, for crystallization of highly textured SrBaNbO on a SrTiO (001) substrate, high heating rate, revealing polycrystalline BaTiO, and atmosphere control with 25% CO, for crystallization of BaTiO. The signal is sufficient to study a single deposited layer (≥10 nm for the crystallized film) which then defines the interface between the substrate and thin film for the following layers. A protocol for processing the data is developed to account for a thermal shift of the entire setup, including the sample, to allow extraction of maximum information from the refinement, e.g. texture. The simplicity of the sample environment allows for the future development of even more advanced measurements during thin-film processing under non-ambient conditions.
了解化学溶液沉积（CSD）法制备的薄膜的结晶过程是设计用于获得高质量器件的制造策略的关键。本文介绍了一种原位样品环境，用于使用近掠入射同步加速器X射线衍射研究CSD法制备的薄膜在典型工艺参数下的结晶情况。通常，热解在快速热处理（RTP）单元中进行，其中高加热速率、高温和气氛控制是主要控制参数。所展示的原位装置能够达到20°C/s的加热速率和1000°C的样品表面温度，与商业RTP单元相当。给出了三个无铅铁电薄膜的例子，以展示新实验装置的潜力：高温下，在SrTiO（001）衬底上结晶高度织构化的SrBaNbO；高加热速率下，揭示多晶BaTiO；25% CO气氛控制下，结晶BaTiO。该信号足以研究单个沉积层（结晶薄膜≥10 nm），这进而定义了后续层的衬底与薄膜之间的界面。开发了一种处理数据的方案，以考虑整个装置（包括样品）的热位移，从而允许从精修中提取最大信息，例如织构。样品环境的简单性为未来在非环境条件下的薄膜加工过程中进行更先进的测量提供了发展空间。
