XRD spectroscopy is an important means of research material inside the crystalline structure of the material. In this study it was analyzed with X-ray sources in terms of manner of preparation of different materials carbon crystal structure of biological characteristics and charring mechanism. The results showed that: Biochar contain d101 and d002 crystal face diffraction peak of carbon graphite-like microcrystalline cellulose, but after charring precipitated salt with different materials, and have a big difference, such as ox dung, castor dregs and furfural dregs of CaCO3 carbon content than other organisms, but only ox dung and castor dregs containing CaMg (CO3)2. Corn stover charcoal preferentially decompose hemicelluloses and cellulose microcrystalline graphite with increasing temperature so with the degree of crystallinity which becomes more stable conversion of carbon compounds. Wherein the mineral salt as a pyrolysis carbonization temperature, gradually precipitated by metals oxides→Acetales→carbonate, and with increasing temperature the content of CaCO3 also increase. After different methods of carbonization, charring its mechanism is different from the first dry charring can promote the decomposition of hemicellulose, high temperature microwave treatment is highly volatile, mainly promoting substances multiple bond rupture decomposed substance carbonate precipitates relatively small. Comprehensive illustrated by X-ray diffraction study biochar may well feature the internal structure of the crystalline, can effectively reflect the cracking mechanism of carbonization process.