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The saturation-free and directionless cross-linking and interpenetration processes between La3+ and [(H2PO4)2Al(HPO4)]-plasma in La–Al phosphate by mixing Al(OH)3, CrO3, and H2O2 dissolved in H3PO4 and La2O3 as a curing accelerator, as well as the thermal stability of the La–Al phosphate bulk materials and the evolutions of the phase composition and morphology at different temperatures were studied using thermogravimetric/differential scanning calorimetry under different temperatures in a muffle furnace. The La–Al phosphates showed good thermal stability, and the thermal weight loss rate of the materials decreased from 18% before heat treatment to ∼2% after heat treatment. In addition, the La–Al phosphate bulk material showed excellent resistance to ablation when subjected to ablation by an oxyacetylene flame at 2000 °C for 30 s. It evolved into a dense LaPO4 and AlPO4 high-temperature phase layer on the sample surface, which prevented further ablation damage to the sample and significantly improved the temperature resistance of the La–Al phosphate bulk material.