Peng Li, Ning Fulong, Li Wei, Sun Jiaxin, Cao Pinqiang, Liu Zhichao, Xie Jingyu
Faculty of Engineering, China University of Geosciences, Wuhan 430074, China.
Laboratory for Marine Mineral Resources, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266237, China.
Scanning. 2019 Oct 17;2019:1694169. doi: 10.1155/2019/1694169. eCollection 2019.
Atomic force microscopy (AFM) indentation is widely used to determine mechanical parameters of various materials. However, AFM tip may lead to phase transition of the cold sample in the region of contact area. It is a long-standing challenge that low-temperature phase-change materials (e.g., ice and hydrate) are hardly characterized by AFM, especially for clathrate hydrates. Here, with theoretical analysis and numerical simulation, we investigated the temperature influence of AFM tip on the tetrahydrofuran (THF) hydrate stability. At first, a steady-state model of heat conduction was established between a v-shaped probe and THF hydrate sample. The temperature of the tip was estimated at different laser spot positions and laser intensities. Through numerical simulation, the heat loss by air convection is less than 1% of the total laser heat, and the influence of ambient air on the AFM probe temperature can be neglected. Meanwhile, the local temperature in the region of contact area was also calculated at the THF hydrate temperature of 0°C, -10°C, -20°C, and -30°C. We found out that the AFM tip causes the cold THF hydrate to melt. The thermal melting thickness decreases with the reduction of laser intensity and THF hydrate temperature. On the contrary, it is positively correlated with the thickness of liquid-like layer on THF hydrate surface and is also linearly increased with the contact radius. This indicates that the thermal melting continues as the press-in depth of the tip into THF hydrate increases. The local temperature rises when the tip touches the THF hydrate. It is easier for THF hydrate to be melted by an external pressure. In addition, the proposed model may be useful for guiding force tests on low-temperature phase-change materials by the AFM indentation.
原子力显微镜(AFM)压痕法被广泛用于测定各种材料的力学参数。然而,AFM探针可能会导致冷样品在接触区域发生相变。低温相变材料(如冰和水合物)很难用AFM进行表征,尤其是对于笼形水合物来说,这是一个长期存在的挑战。在此,通过理论分析和数值模拟,我们研究了AFM探针温度对四氢呋喃(THF)水合物稳定性的影响。首先,建立了V形探针与THF水合物样品之间的稳态热传导模型。在不同激光光斑位置和激光强度下估算了探针的温度。通过数值模拟发现,空气对流造成的热损失小于激光总热量的1%,因此可以忽略环境空气对AFM探针温度的影响。同时,还计算了在THF水合物温度为0°C、-10°C、-20°C和-30°C时接触区域的局部温度。我们发现AFM探针会使冷的THF水合物融化。热融化厚度随激光强度和THF水合物温度的降低而减小。相反,它与THF水合物表面类液层的厚度呈正相关,并且也随接触半径线性增加。这表明随着探针压入THF水合物深度的增加,热融化会持续进行。当探针接触THF水合物时,局部温度会升高。THF水合物在外压作用下更容易融化。此外,所提出的模型可能有助于指导通过AFM压痕法对低温相变材料进行力测试。