4826-71-5 Purity
98%
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Specification
Zirconium tungstate (ZrW2O8) was synthesized by the amorphous citrate method, where the citrate gel was prepared from zirconium oxide nitrate [ZrO(NO3)2·xH2O], ammonium metatungstate [(NH4)6W12O39·xH2O] and citric acid (CA) aqueous solution.
Synthesis procedure
· Due to the unclear composition of crystal water in zirconium dinitrate oxide and ammonium metatungstate, specific amounts of each were heated to temperatures of 900 °C and 600 °C, respectively, to convert them into ZrO2 and WO3.
· Two separate solutions of the above metal salts were created; when combined, these produced a solution with zirconium and tungsten in the stoichiometric ratio of ZrW2O8, each at a concentration of 0.1 M with respect to the metal.
· Anhydrous CA was then added to the zirconium dinitrate oxide solution while stirring continuously, maintaining a CA to metal molar ratio of 2:1. A white precipitate formed immediately but dissolved after several minutes.
· The quantity of CA added to the ammonium metatungstate solution was adjusted to achieve molar ratios of CA to total metal cations of 1.33, 1, and 0.66 upon mixing the two solutions. The pH of the resulting mixture was found to be between 1.1 and 1.2 and was later adjusted to around pH 10 by introducing a 25% aqueous ammonia solution.
· The resulting clear and colorless solution was concentrated in a rotary evaporator under vacuum at 70 °C until achieving a sufficiently low viscosity for flask removal. Finally, the concentrated solution was transferred into dishes and dried for 20 hours at 85 °C. Thermolysis of the resultant gels was conducted in a muffle furnace with a vented heating chamber, employing various heating protocols.
From the solution of ammonium cerium (IV) nitrate and zirconium oxide nitrate, single enzyme biomineralization generated ceria and ceria zirconia solid solution nanocrystals (less than 3 nm in diameter). The nanocrystals produced were active catalysts for carbon monoxide oxidation for environmental use.
Synthesis procedure of nanoparticles
· Modified silicatein was generated from E coli BL21(DE3) pLysS cells by isopropyl -D-1-thiogalactopyranoside (IPTG) induction and isolated by immobilised metal affinity chromatography (IMAC).
· The particle synthesis was initiated by adding the following to the filtered protein solution (4 M silicatein): (i) 2 mM cerium ammonium nitrate, (ii) 2 mM zirconium dinitrate oxide hydrate [ZrO(NO3)2·xH2O], (iii) a solution of 1 mM cerium ammonium nitrate and 1 mM zirconium dinitrate oxide hydrate.
· The samples were heated on an orbital shaker. They were 24 hours later centrifuged for 10 minutes at 18,000 G and the pellet was rinsed again in 2 mM nitric acid. It was this washing-up that was five times. Zeta potential of ceria nanoparticles decreases with increasing pH which allows for stable nanoparticle solution in dilute nitric acid without the need for another capping agent. They were centrifuged and vacuum dried at intervals before catalytic testing and structural characterisation.