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SThM-based local thermomechanical analysis: Measurement intercomparison and uncertainty analysis
International Journal of Thermal Sciences ( IF 4.5 ) Pub Date : 2020-10-01 , DOI: 10.1016/j.ijthermalsci.2020.106502
Eloise Guen , Petr Klapetek , Robert Puttock , Bruno Hay , Alexandre Allard , Tony Maxwell , Pierre-Olivier Chapuis , David Renahy , Guillaume Davee , Miroslav Valtr , Jan Martinek , Olga Kazakova , Séverine Gomès

Abstract We assess Scanning Thermal Microscopy (SThM) with a self-heated doped silicon nanoprobe as a method for determining the local phase transition temperature of polymeric materials by means of nano-thermomechanical analysis (nano-TA). Reference semi-crystalline samples and amorphous test samples, characterized first using differential scanning calorimetry (DSC), are studied by nano-TA in the temperature range 50–250 °C. The repeatability, the reproducibility and the reliability of nano-TA are evaluated by three laboratories by applying the same calibration protocol prior to and after the measurements. The calibration of the probe temperature scale and the variability of the sample thermomechanical response are validated by Monte Carlo uncertainty analysis, resulting in a calculated uncertainty between 3 and 5 K. The SThM probe temperature data represented as a function of DSC-measured phase-transition temperatures of the semi-crystalline samples rule out the possibility of a quadratic fit and call for a linear calibration in absence of additional information. The maximum deviation obtained between SThM and DSC temperatures with such linear calibration reaches ± 30 K for melting temperatures and 50 K for glass transition temperatures.

中文翻译:

基于 SThM 的局部热机械分析:测量比对和不确定度分析

摘要 我们评估了使用自加热掺杂硅纳米探针的扫描热显微术 (SThM) 作为一种通过纳米热机械分析 (nano-TA) 确定聚合物材料局部相变温度的方法。参考半结晶样品和无定形测试样品,首先使用差示扫描量热法 (DSC) 进行表征,通过纳米 TA 在 50-250 °C 的温度范围内进行研究。三个实验室通过在测量前后应用相同的校准协议来评估纳米 TA 的可重复性、再现性和可靠性。探针温标的校准和样品热机械响应的可变性通过蒙特卡罗不确定性分析进行验证,导致计算出的不确定性介于 3 和 5 K 之间。SThM 探针温度数据表示为半结晶样品的 DSC 测量相变温度的函数,排除了二次拟合的可能性,并在没有附加信息的情况下要求进行线性校准。使用这种线性校准在 SThM 和 DSC 温度之间获得的最大偏差对于熔化温度达到 ± 30 K,对于玻璃化转变温度达到 50 K。
更新日期:2020-10-01
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