Dispersion and distribution of titanium species bound to silica from titanium tetrachloride

Haukka, Suvi; Lakomaa, Eeva Liisa; Jylhä, O.; Vilhunen, J.K.; Hornytzkyj, Seppo

doi:10.1021/la00036a026

Cited by 122 publications

(148 citation statements)

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“…1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 The core-shell spheres structure of the aggregate nanoparticles of Si 5 (PO 4 ) 6 O/SiO 2 was possible to observe clearly in the case of pyrolysis of precursor (3), as is shown in figures 4e,f. For all the cases the core-shell structure was also corroborated from energy dispersive X-Ray spectroscopy data and using a method previously reported 30,31 based on the core/shell contents in this case, from the Si/P contents at of SiO 2 spheres coated with Si 5 (PO 4 ) 6 O. As is ilustrated for the pyrolyt...…”

Section: Scheme 3 Schematic Representation Of the Distribution Of Prosupporting

confidence: 60%

“…The reaction of N 3 P 3 Cl 6 with H 2 N(CH 2 ) 3 Si(OEt) 3 31 P NMR spectrum for the compound (2) showed two resonances at 20.8 ppm. and 17.97 ppm(both nearly multiplets) with a relative intensity of 1:2, see supporting information , S 2 .…”

Section: Synthesis Of the Precursorsmentioning

confidence: 99%

“…Financial support from FONDECYT, project 1085011, is also acknowledged. 31 P NMR spectrum for (1) , (2) and (3) and TGA curves for (2) and (3) in air and N 2 and DSC curves for (1) , (2) and (3) in air and nitrogen.…”

Section: Acknowledgementsmentioning

confidence: 99%

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Synthesis and Characterization of Cyclotriphosphazenes Containing Silicon as Single Solid-State Precursors for the Formation of Silicon/Phosphorus Nanostructured Materials

et al. 2008

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The synthesis and characterization of new organosilicon derivatives of N 3 P 3 Cl 6 , N 3 P 3 [NH(CH 2 ) 3 Si(OEt) 3 ] 6 (1),Pyrolysis of 1, 2, and 3 in air and at several temperatures results in nanostructured materials whose composition and morphology depend on the temperature of pyrolysis and the substituents of the phosphazenes ring. The products stem from the reaction of SiO 2 with P 2 O 5 , leading to either crystalline Si 5 (PO 4 ) 6 O, SiP 2 O 7 or an amorphous phase as the glass Si 5 (PO 4 ) 6 O/3SiO 2 • 2P 2 O 5 , depending on the temperature and nature of the trimer precursors. From 1 at 800 °C, core-shell microspheres of SiO 2 coated with Si 5 (PO 4 ) 6 O are obtained, while in other cases, mesoporous or dense structures are observed. Atomic force microscopy examination after deposition of the materials on monocrystalline silicon wafers evidences morphology strongly dependent on the precursors. Isolated islands of size ∼9 nm are observed from 1, whereas dense nanostructures with a mean height of 13 nm are formed from 3. Brunauer-Emmett-Teller measurements show mesoporous materials with low surface areas. The proposed growth mechanism involves the formation of cross-linking structures and of vacancies by carbonization of the organic matter, where the silicon compounds nucleate. Thus, for the first time, unique silicon nanostructured materials are obtained from cyclic phosphazenes containing silicon.

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Section: Scheme 3 Schematic Representation Of the Distribution Of Prosupporting

confidence: 60%

Section: Synthesis Of the Precursorsmentioning

confidence: 99%

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Synthesis and Characterization of Cyclotriphosphazenes Containing Silicon as Single Solid-State Precursors for the Formation of Silicon/Phosphorus Nanostructured Materials

et al. 2008

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“…With increasing reaction temperature of TiCl 4 and SiO 2 , the intensities of Raman bands due to TiO 2 (anatase) increase remarkably. This is because the agglomeration of TiO 2 and chlorination of OH groups of silica by HCl occurs at high grafting temperatures [21]. At lower reaction temperatures, amorphous TiO 2 was the dominant species on the surface of silica [29].…”

Section: Characterization Of Ti/sio 2 (T)mentioning

confidence: 99%

“…In principle, it is possible to prepare the highly isolated titanium ions on SiO 2 if the SiO 2 is partially dehydroxylated beforehand. The reaction of TiCl 4 with silica has been well studied by various spectroscopies to determine the species formed [21][22][23]. In general, TiCl 4 can react with SiO 2 surface as follows:…”

Section: Introductionmentioning

confidence: 99%