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High-sensitivity differential scanning calorimetry using a MEMS thermopile chip for analyzing polymer crystallization
Zechun Li1,2, Shaokui Tan1,3, Ming Li1,2
1State Key Lab of Transducer Technology, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050, China. xpc@mail.sim.ac.cn.
The Analyst
|April 7, 2025
Summary
A novel high-sensitivity differential scanning calorimetry (DSC) technique using a MEMS chip analyzes polyamide 6 (PA6) crystallization. This method reveals critical rates for melt and cold crystallization, and phase transitions, enabling detailed thermal behavior studies.
Area of Science:
- Materials Science
- Polymer Science
- Analytical Chemistry
Background:
- Differential Scanning Calorimetry (DSC) is crucial for material thermal analysis.
- Existing DSC techniques face limitations in sensitivity and speed for rapid thermal processes.
- Understanding polymer crystallization kinetics is vital for material performance.
Purpose of the Study:
- To introduce a high-sensitivity MEMS-based DSC technique for advanced thermal analysis.
- To investigate the crystallization behavior of polyamide 6 (PA6) under diverse thermal conditions.
- To establish critical rates for PA6 melt-crystallization, cold-crystallization, and phase transitions.
Main Methods:
- Development and application of a MEMS single-crystalline silicon thermopile chip for DSC.
- Utilizing the chip to perform non-isothermal and isothermal experiments on PA6.
- Analysis of exothermic signals for phase transitions and crystallization kinetics.
Main Results:
- The MEMS DSC chip exhibits high temperature and power responsivity with a fast cooling time constant.
- Identified critical cooling rate of 50 °C s⁻¹ for suppressing PA6 melt-crystallization.
- Determined critical heating rate of 300 °C s⁻¹ for suppressing PA6 cold-crystallization.
- Detected subtle γ-α phase transition in PA6 at a critical heating rate of 25 °C s⁻¹.
- PA6 crystallization observed between 70 °C and 170 °C, with a shortest half-crystallization time of ~1.1 s at 120 °C.
Conclusions:
- The developed high-sensitivity MEMS DSC technique accurately characterizes PA6 crystallization kinetics and phase transitions.
- The technique is suitable for studying materials under high heating and cooling rates.
- This advancement offers significant potential for material science research and development.
