Nguyen Long Quang, Larsen Peter Emil, Larsen Tom, Goswami Sanjukta Bose, Villanueva Luis Guillermo, Boisen Anja, Keller Stephan Sylvest
1DNRF and Villum Fonden Center for Intelligent Drug Delivery and Sensing Using Microcontainers and Nanomechanics, IDUN, Technical University of Denmark, 2800 Kgs Lyngby, Denmark.
2DTU Nanolab, Technical University of Denmark, 2800 Kgs Lyngby, Denmark.
Microsyst Nanoeng. 2019 Oct 21;5:58. doi: 10.1038/s41378-019-0094-x. eCollection 2019.
Thermal analysis is essential for the characterization of polymers and drugs. However, the currently established methods require a large amount of sample. Here, we present pyrolytic carbon resonators as promising tools for micromechanical thermal analysis (MTA) of nanograms of polymers. Doubly clamped pre-stressed beams with a resonance frequency of 233 ± 4 kHz and a quality factor (Q factor) of 800 ± 200 were fabricated. Optimization of the electrical conductivity of the pyrolytic carbon allowed us to explore resistive heating for integrated temperature control. MTA was achieved by monitoring the resonance frequency and quality factor of the carbon resonators with and without a deposited sample as a function of temperature. To prove the potential of pyrolytic carbon resonators as thermal analysis tools, the glass transition temperature ( ) of semicrystalline poly(L-lactic acid) (PLLA) and the melting temperature ( ) of poly(caprolactone) (PCL) were determined. The results show that the of PLLA and of PCL are 61.0 ± 0.8 °C and 60.0 ± 1.0 °C, respectively, which are in excellent agreement with the values measured by differential scanning calorimetry (DSC).
热分析对于聚合物和药物的表征至关重要。然而,目前已确立的方法需要大量样品。在此,我们展示了热解碳谐振器作为用于纳克级聚合物微机械热分析(MTA)的有前景的工具。制造出了具有233±4kHz共振频率和800±200品质因数(Q因子)的双端固支预应力梁。热解碳电导率的优化使我们能够探索用于集成温度控制的电阻加热。通过监测有和没有沉积样品时碳谐振器的共振频率和品质因数随温度的变化来实现MTA。为了证明热解碳谐振器作为热分析工具的潜力,测定了半结晶聚(L-乳酸)(PLLA)的玻璃化转变温度()和聚己内酯(PCL)的熔点()。结果表明,PLLA的和PCL的分别为61.0±0.8°C和60.0±1.0°C,这与差示扫描量热法(DSC)测得的值非常吻合。