An Integrated Hardware–Software Platform for Automated Thermodynamic Characterization of Gas–Solid Interfaces Using a Resonant Microcantilever

Measurement of material thermodynamic parameters plays a crucial role in understanding the interactions between host materials and guest species. Therefore, developing a general-purpose system for thermodynamic parameter measurement is of great significance. In this work, a complete gas–solid interface thermodynamic parameter measurement platform was developed based on isothermal adsorption and a resonant microcantilever testing platform. Unlike conventional adsorption measurement systems that rely on manual, multi-cycle adsorption–desorption processes, the proposed platform integrates an automated hardware–software architecture together with a stepwise concentration-gradient protocol and on-chip thermal desorption, enabling continuous and efficient acquisition of adsorption isotherms. The study includes: (i) construction of an improved thermodynamic parameter extraction model based on the Sips model, (ii) development of an integrated resonant microcantilever control and acquisition module using a modified Fourier algorithm, and (iii) implementation of an automated testing and data analysis software framework developed in LabVIEW based on the Queued Message Handler (QMH) architecture. The system was validated from both hardware performance and material testing perspectives using CO2 adsorption on H-SSZ-13 as a representative case. The results show that the system achieves a maximum sampling rate of 10,000 pts (points per second), with minimum root-mean-square (RMS) noise levels of 0.0083 Hz for frequency and 0.0109 °C for temperature. The PID temperature-control settling time (0.1%) is 24.9 ms, and the frequency-response settling time (0.01%) is 9.6 ms. Thermodynamic parameters including entropy change (ΔS), enthalpy change (ΔH), and Gibbs free energy change (ΔG) were successfully extracted during CO2 adsorption at 294.15 K under different relative uptakes. Reproducibility was verified across three independent samples, yielding a standard deviation of 9.1 J·mol−1 for ΔS at 2% relative uptake and relative standard deviations of 6.85% and 8.12% for ΔH and ΔG, respectively. These results demonstrate that the proposed thermodynamic measurement platform features a simple architecture, superior performance, and high reproducibility in gas–solid interface thermodynamic studies, showing strong potential for future commercialization.