A gel material that can be applied to industry needs to fulfill two requirements: excellent mechanical properties and high temperature resistance. Previous research developed a hydrogel enhanced by sub‐5 nm particles, with excellent mechanical properties. While its application in the open environment is still limited by the volatilization of inner moisture, in this research, a non‐volatile gel (NV gel) enhanced by 5‐nm spherulites is manufactured. The NV gel remains stable after staying at 90 °C for 24 h. Meanwhile, being enhanced by sub‐5 nm nanospherulites, the NV gel shows good mechanical properties: with 200 ppm nanoparticle content, the tensile strength reaches 814 kPa and the compressive stress is 173.41 MPa at a recoverable 99% strain. The high temperature resistance is characterized by thermogravimetric analysis (TGA) and mechanical testing after thermal treatment. Transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, time of flight secondary ion mass spectrometry, and thermogravimetric analysis are used to evaluate the microstructure of NV gel. Possessing non‐volatile and good mechanical properties at the same time, this NV gel becomes very suitable for fulfilling the application requirement as an engineering material.