Detailed studies on the preparation of crystalline α-zirconium phosphate (α-ZrP), polyaniline (PANI) -intercalated α-ZrP composition and PANI/α-ZrP nanocomposite are presented. The crystal structure, composition and morphology of a-ZrP, PAN-intercalated a-ZrP composition and PANI/a-ZrP nanocomposite, the synthesis conditions of a-ZrP, reaction process of in suit chemical polymerization of aniline and electrochemical properties of polyaniline (PANI) -intercalated α-ZrP composition and PANI/α-ZrP nanocomposite are characterized by means of X-ray diffraction (XRD), Inductive coupled plasma emission spectrometry (ICP), Fourier transform infrared (FT-IR), Thermogravimetry/differential thermal analysis-evolved gas mass Field-emission scanning electromicroscope (FESEM), Atomic force microscope (AFM) and electrochemical testing.
The crystalline α-ZrP with a narrow lateral size distribution is synthesized by a reformative hydrothermal method involving separate nucleation and hydrothermal aging steps. Two solutions are added simultaneously to a colloid mill, uniform and fine crystal is formed and then the resulting slurry is transferred rapidly from the reactor to a Teflon-lined stainless steel autoclave and ages at a certain temperature for a certain time. In order to control the lateral size and crystallinity of α-ZrP, various parameters such as the concentration of zirconium ion, phosphoric acid, hydrochloric acid, reaction temperature and reaction time are systematically studied by orthogonal design of experiments. The concentration of phosphoric acid and reaction temperature are the major parameters for crystallinity while the reaction temperature and concentration of zirconium are the most important factors for lateral size of a-zirconium phosphate