Conte Marcello, Mohanty Gaurav, Schwiedrzik Jakob J, Wheeler Jeffrey M, Bellaton Bertrand, Michler Johann, Randall Nicholas X
Anton Paar TriTec SA, Rue de la Gare 4, Peseux 2034, Switzerland.
Laboratory for Mechanics of Materials and Nanostructures, Empa-Swiss Federal Laboratories for Materials Science and Engineering, Feuerwerkerstrasse 39, Thun 3602, Switzerland.
Rev Sci Instrum. 2019 Apr;90(4):045105. doi: 10.1063/1.5029873.
High temperature nanoindentation is an emerging field with significant advances in instrumentation, calibration, and experimental protocols reported in the past couple of years. Performing stable and accurate measurements at elevated temperatures holds the key for small scale testing of materials at service temperatures. We report a novel high temperature vacuum nanoindentation system, High Temperature Ultra Nanoindentation Tester (UNHT HTV), utilizing active surface referencing and non-contact heating capable of performing measurements up to 800 °C. This nanoindenter is based on the proven Ultra Nano-Hardness Tester (UNHT) design that uses two indentation axes: one for indentation and another for surface referencing. Differential displacement measurement between the two axes enables stable measurements to be performed over long durations. A vacuum level of 10 mbar prevents sample surface oxidation at elevated temperatures. The indenter, reference, and sample are heated independently using integrated infrared heaters. The instrumental design details for developing a reliable and accurate high temperature nanoindenter are described. High temperature calibration procedures to minimize thermal drift at elevated temperatures are reported. Indentation data on copper, fused silica, and a hard coating show that this new generation of instrumented indenter can achieve unparalleled stability over the entire temperature range up to 800 °C with minimum thermal drift rates of <2 nm/min at elevated temperatures.
高温纳米压痕是一个新兴领域，在过去几年中，该领域在仪器设备、校准和实验方案方面都取得了重大进展。在高温下进行稳定而准确的测量是在服役温度下对材料进行小规模测试的关键。我们报告了一种新型的高温真空纳米压痕系统——高温超纳米压痕测试仪（UNHT HTV），它利用有源表面参考和非接触加热技术，能够在高达800°C的温度下进行测量。这种纳米压痕仪基于经过验证的超纳米硬度测试仪（UNHT）设计，该设计使用两个压痕轴：一个用于压痕，另一个用于表面参考。两个轴之间的差分位移测量使得能够长时间进行稳定测量。10毫巴的真空度可防止样品表面在高温下氧化。压头、参考物和样品使用集成红外加热器独立加热。本文描述了开发可靠且准确的高温纳米压痕仪的仪器设计细节。报告了用于最小化高温下热漂移的高温校准程序。对铜、熔融石英和硬涂层的压痕数据表明，这种新一代的仪器化压痕仪在高达800°C的整个温度范围内能够实现无与伦比的稳定性，在高温下的最小热漂移率<2纳米/分钟。
