1：Experimental Design and Method Selection:

A facile low-temperature solution process using Li-ethylenediamine (Li-EDA) as a reducing agent was employed to reduce Ti3C2Tx multilayers. Techniques included X-ray photoelectron spectroscopy (XPS), electron spin resonance (ESR), magnetization measurements, X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), and thermogravimetric analysis (TGA).

2：Sample Selection and Data Sources:

Ti3AlC2 was synthesized from Ti2AlC and TiC powders, then etched with HF to produce Ti3C2Tx. Reduction was performed at temperatures of 25, 40, 80, and 120 °C.

3：List of Experimental Equipment and Materials:

Equipment included FE-SEM (JSM-6701F/INCA Energy, JEOL), TEM (JEOL JEM 3010), AFM (SPA400 with SPI-3800 controller, Seiko Instrument Industry Co.), XRD (Rigaku Ultima IV), XPS (Thermo VG Microtech ESCA 2000), Raman spectrometer (Renishaw RM1000-In Via), TGA (Polymer laboratory TGA 1000 plus), ESR spectrometer (Bruker EMX plus 6/1), SQUID magnetometer, and VSM. Materials included Ti2AlC (Kanthal), TiC (Alfa Aesar), Li metal (Sigma Aldrich), EDA (Sigma Aldrich), HF, DI water, ethanol.

4：Experimental Procedures and Operational Workflow:

Ti3AlC2 was synthesized by ball milling and heating, then etched with HF. Reduction involved mixing Ti3C2Tx with Li and EDA under N2 atmosphere at specified temperatures, followed by washing with water and ethanol. Delamination was achieved by sonication and filtration.

5：Data Analysis Methods:

XPS spectra were analyzed for oxidation states, ESR for paramagnetic signals, magnetization data for susceptibility calculations, and other techniques for structural and chemical characterization.