Controllable Synthesis Of Crystalline α-Zirconium Phosphate And The Preparation And Property Of Its Composition Materials

Detailed studies on the preparation of crystallineα-zirconium phosphate(α-ZrP), polyaniline(PANI)-intercalatedα-ZrP composition and PANI/α-ZrP nanocomposite are presented. The crystal structure, composition and morphology ofα-ZrP, PANI-intercalatedα-ZrP composition and PANI/α-ZrP nanocomposite, the synthesis conditions ofα-ZrP, reaction process of in suit chemical polymerization of aniline and electrochemical properties of polyaniline(PANI)-intercalatedα-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 spectrometry(TG/DTA-EGMS), Field-emission scanningelectromicroscope(FESEM), Atomic force microscope(AFM) and electrochemical testing.The crystallineα-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 ofα-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 ofα-zirconium phosphate.The controlled chemical oxidative polymerization of aniline(ANI) monomer within the interlayer ofα-ZrP is performed by the use of ferric trichloride as an oxidant. The reaction process of oxidative polymerization of ANI monomer between the layers ofα-ZrP is interpreted as follows: upon the addition of oxidant, Fe³⁺ enters into the layer by ion-exchange and initiates the oxidative polymerization of the interlayer monomer. The XRD partner indicates that the product is PANI-intercalatedα-ZrP composition. The electrochemical property of PANI-intercalatedα-ZrP composition is studied by AC Impedance technique and its conductivity is 4.49×10⁽-59S/cm.The synthesis process of PANI/α-ZrP nanocomposite is:α-ZrP nanosheet is exfoliated by tetramethyl ammonium hydroxide (TMAOH), then PANI/α-ZrP nanocomposite is synthesized from the oxidant of ANI which is dispersed in theα-ZrP nanosheet solution. The AFM imagines indicate the structure ofα-ZrP nanosheet. The XRD pattern indicates thatα-ZrP nanosheet homodisperse in PANI. The electrochemical property of PANI/α-ZrP nanocomposite is studied by AC Impedance technique and its conductivity is 6.86×10^-6 S/cm.