Three kinds of novel diatomite/ground calcium carbonate composite humidity control materials were prepared with different calcination temperatures using diatomite and ground calcium carbonate (GCC) as raw materials. The microstructure and morphology properties of samples were studied by nitrogen gas adsorption, mercury intrusion porosimetry (MIP) and fractal dimensions on the basis of gas adsorption isotherms with FHH methods. Fourier transform infrared spectroscope (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the mineral composition and surface properties. Furthermore, X-ray diffraction (XRD), thermo-gravimetry and differential scanning calorimetry (TG-DSC) were used to analyze the formation mechanism of composite material. It was indicated that DG750 showed the better moisture adsorption performance. The 72 h moisture adsorbed amount of DG750 reached 11.66%, 8.81% and 8.00% at 98%RH, 85%RH and 75%RH, respectively, which improved about 0.46, 0.54 and 0.53-fold as those of diatomite. The hydrophilic calcium silicate, calcium oxide and calcium hydroxide were formed in the DG750 during the calcinations process. As compared with the raw materials, the content of mesoporous component increases in the DG750, which is in favor of capillary condensation and improving moisture adsorption ability. (C) 2017 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.