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For the doping elements, the semi-core states 4d or 4s and 4p or 2p were included for indium, yttrium and magnesium. The basic set used for the doping elements was as follows: Sn: 5s, 5p, 6s, 6p, 7s Sb: 5s, 5p, 6s, 6p, 7s In: 4d, 5s, 5p, 6s, 6p, 7s Ge: 4s,4p,4d Y: 4s, 4p, 4d, 5s, 5p Nb: 4s, 4p, 4d, 5s, 5p F: 2s,2p Mn: 3d, 4s, 4p Cu: 3d, 4s, 4p Mo: 4s, 4p, 4d, 5s, 5p Cd: 4d, 5s, 5p, 6s, 6p Ce: 4f, 5s, 5 p, 6s, 6p, 7s, 7p, 8s W: 5d, 6s, 6p Bi: 6s, 6p, 7s, 7p, 8s Mg: 2p, 3s, 3p Al: 3s, 3p The kinetic energy cut-off for the plane waves was eV.
Structural geometric optimisation was not performed, since the mathematical model could be evaluated and confirmed on the basis of known experimental results coating with Sn, Al, Zr and Zn. Thus, the model calculations yield sufficient accuracy for examination of the photostability. The state density calculations were based on a grid according to the Monkhorst-Pack scheme. The surface calculations were performed in accordance with the "slab model method" with a vacuum thickness of 10 A.
In this context, the unit cell comprises 52 atoms Ti 8 Si 8 0 3. Applied to the pigment, the calculated monomolecular coverage with SiO 2 with a layer thickness of approximately 0.
The percentage by weight was calculated on the basis of the following values: typical value of the specific surface to BET for TiO 2 particles manufactured by the chloride process: 6. Examples 1 to 14 and Reference Example 2 and 3 describe coverage of the TiO 2 surface with a monomolecular SiO 2 layer doped at an atomic ratio of 1 doping element X : 7 Si , i.
Applied to the TiO 2 pigment, this results in the following percentages by weight of the doping elements, calculated as oxide and referred to TiO 2 : Example 1: roughly 0. This can be analysed in the form of band structures energy bands spatially resolved or the state densities integrated energy states.
Figure 1 shows a simplified block diagram d of the electronic structure. The block diagram reflects only the energy bandwidth and position of the energy band.
The state density e is used for the energy state distribution within the energy band. Figure 2 shows the effect of a pure, undoped SiO 2 coating Reference Example 1 on the photoactivity of the TiO 2 : the calculated state density of the pure TiO 2 surface is shown as a broken line, that of the Si0 2 -coated surface as a solid line.
The positive effect of the SiO 2 coating on photostability is partly based on the reduction of the state density near the band edge in the conduction band CB , compared to the uncoated TiO 2 surface, this reducing the transfer of electron-hole pairs to the surrounding matrix.
At the same time, the positive effect is intensified by the fact that there is additionally a reduction in the state density near the band edge in the valence band VB. Figure 3 shows the effect of doping the SiO 2 layer with Sn Example 1 on the state densities, compared to the pure Si0 2 coating. In this case, there is a further reduction in the VB state density, this leading to improved photostability.
Surprisingly, a reduction in the VB state density near the band edge can be seen in each case, meaning that these coatings lead to an increase in photostability.
Similar doping of the Si0 2 layer with the elements Zr or Zn likewise leads to improved stability compared to an undoped Si0 2 layer. Figure 17 shows the effect of doping the Si0 2 layer with Mg Reference Example 2 on the state densities. In this case, there is an increase in the VB state density, meaning that doping of the SiO 2 layer with Mg results in a loss of photostability.
Figure 18 shows the effect of doping the Si0 2 layer with Al Reference Example 3 on the state densities. In this case, there is likewise an increase in the VB state density, meaning that doping of the Si02 layer with Al results in a loss of photostability. The results of the state density calculations correlate favourably with the data of photostability determined with experimentally doped samples. Thus, by means of the calculation method described useful doping elements for increasing the photostability of TiO 2 pigments with dense SiO 2 skin dense skin pigments can be predicted more precisely than by means of the "trial and error method" of chemical experiments.
Based on the present invention the person skilled in the art may calculate and predict the suitability of further doping elements or combinations of doping elements for improvement of the photostability of dense-skin pigments which have not been mentioned in the prior art or in this specification. Process control Methods for coating titanium dioxide particles with dense SiO 2 as such are known.
The traditional processes work via the aqueous phase. To this end, a TiO 2 particle suspension is produced, mixed with a dispersant where appropriate, and wet-milled where appropriate. The dense Si0 2 skin is customarily precipitated by adding alkali metal-silicate solutions and appropriate pH value control.
The doping element is added in the form of a salt solution, together with the silicate solution or separately before or after addition of the silicate solution.
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