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An experimental binary phase diagram of 2-Amino-2-methyl-1, 3-propanediol (AMPL)-tris(hydroxymethyl)aminomethane (TRIS) is developed by using high temperature in-situ X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermodynamics modeling. The organic thermal energy storage materials, such as AMPL and TRIS, undergo a solid–solid state phase transition storing large amounts of thermal energy in O–H…O and O–H…N bond rotation. High temperature in-situ XRD and DSC experiments are used to study binary equilibrium AMPL-TRIS phase diagram. Binary solid solutions of AMPL and TRIS exhibit an orientationally disordered BCC structure, in which thermal energy is stored. A computer developed AMPL-TRIS phase diagram by CALPHAD methodology agrees reasonably well with the experimental one. Gibbs energies of pure components were described based on their heat …