第五讲ApplicationofXRD-examples.pptVIP

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第五讲ApplicationofXRD-examples.ppt

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第五讲ApplicationofXRD-examples

Example I--Alteration of aggregates XRD物相分析及其应用物相分析原理应用案例无机矿物材料高分子材料金属材料 LDH Based on the structure of Brucite (Mg(OH)2) Substitution of Mg(II) by trivalent cations of similar size Formation of positive metallic layers (brucite layers) Excess of positive charges are neutralized by inter layer anions Water of crystallization is found between the layers Uses and Possible Applications of LDH Adsorbents, catalysts ,catalyst precursors1,2 anionic exchangers3 electrochemistry4 Material for the positive electrode in Ni-Cd, NiMH batteries Microporous and mesoporous materials5 Separation membranes having high temperature stability LDH materials, and intercalation a) Synthesis of the LDHs Co-precipitation typically Zn:Al: ratio: 2:1, 3:1, 4:1 b) LDH intercalation compounds (PPA for example) LDH is added to a 0.1 M solution of phenyl phosphonic acid (PPA) solution Heated for 48 hrs at 70°C Mixture is filtered, rinsed and dried for 18 hrs at 70°C Powder XRD From the XRD pattern we can determine the interlayer spacing of the material (00l line) An increase in the interlayer spacing indicates a successful reaction Interlayer Spacing of the Materials d spacing similar to pure zirconium phenyl phosphonates (ca 14.7 ?) Increase in d spacing confirms successful reaction Example IIIOrgano-Clay and its composites * Kingston, Canada XRD of the surface of Spratt limestone NaOH KOH LiOH Ref. XRD of the surface of Pittsburg limestone Example II Hydrotalcites; Layered Double Hydroxides (LDH) OH- OH- CO32- H2O M(II), M(III) Structure General Formula of a LDH [M2+(1-x)M3+x(OH)2][An-]x/n?zH2O M2+ = Mg2+, Zn2+, Ni2+, etc. M3+ = Al3+, Ga3+, Co3+, etc. 0.17 x 0.33 5:1 M2+:M3+ 2:1 An- = CO32-, Cl-, NO3-, phenyl phosphonate, benzoate, POM anions (i.e. H2W12O406-) 1) Cavani, F.; Trifiro, F.; Vaccari, A. Catal.Today 1991, 11, 173-301. 2) Kruissink E.C.; Van Reijen L.L. J.Chem.Soc.Faraday Trans. 1981, 77 , 649-663. 3) Meyn, M.; Beneke, K.; Lagaly, G. Inorg.Ch