Iron-silicon oxide particles having an improved heating rate in an alternating magnetic and electromagnetic field
View Patent ↗Iron-silicon oxide particles with a core and an outer shell have improved heating rates in a magnetic field. The core contains maghemite, magnetite, and haematite. The outer shell is essentially or exclusively silicon dioxide. The crystallite diameter of the haematite determined by X-ray diffraction is greater than 120 nm. A ratio of the brightness of the Debye-Scherrer diffraction ring by electron diffraction at a lattice plane spacing of 0.20+/−0.02 nm, comprising maghemite and magnetite, to the brightness of the Debye-Scherrer diffraction ring by electron diffraction at a lattice plane spacing of 0.25+/−0.02 nm, comprising maghemite, magnetite and haematite, is no more than 0.2.
1. An iron-silicon oxide particle, comprising:
a core and
an outer shell,
wherein the core comprises maghemite, magnetite, and haematite, as iron oxide modifications,
the outer shell consists essentially or exclusively of amorphous silicon dioxide,
the particle satisfies:
B 0.20 nm /B 0.25 nm is ≦0.2,
B 0.20 nm is brightness of a Debye-Scherrer diffraction ring determined by electron diffraction at a lattice plane spacing of 0.20+/−0.02 nm, comprising maghemite and magnetite,
B 0.25 nm is brightness of a Debye-Scherrer diffraction ring determined by electron diffraction at a lattice plane spacing of 0.25+/−0.02 nm, comprising maghemite, magnetite and haematite, and
a crystallite diameter of the haematite determined by X-ray diffraction is greater than 120 nm.
2. The iron-silicon oxide particle according to claim 1 ,
wherein a crystallite diameter of haematite and a crystallite diameter of magnetite are each independently more than 120 nm and
a crystallite diameter of maghemite is not more than 70 nm.
3. The iron-silicon oxide particle according to claim 1 , further comprising a partially or fully formed inner shell between the core and the outer shell,
wherein the inner shell comprises iron, silicon, and oxygen,
the inner shell has a spacing of lattice planes of 0.31+/−0.02 nm in HR-TEM, and
the inner shell has a thickness of less than 2 nm.
4. The iron-silicon oxide particle according to claim 1 , wherein an iron oxide content of the particle, calculated as Fe 2 O 3 , is from 60 to 95% by weight.
5. The iron-silicon oxide particle according to claim 1 , wherein a BET surface area of the particle is from 5 to 50 m 2 /g.
6. The iron-silicon oxide particle according to claim 1 , wherein an average degree of branching of aggregates is at least 7.
7. The iron-silicon oxide particle according to claim 6 , wherein an average length of branches of an aggregate is at least 500 nm.
8. The iron-silicon oxide particle according to claim 1 , obtained by a process comprising modifying by adsorption, reaction on a surface, or complexation of or with organic and inorganic reagents.
9. A process for producing the iron-silicon oxide particle of claim 1 , the process comprising:
igniting and reacting a mixture comprising from 0 to 30% of a total amount of at least one hydrolysable or oxidizable or both hydrolyzable and oxidizable silicon compound, an oxidizable or hydrolysable or both oxidizable and hydrolyzable iron compound, a hydrogen-containing fuel gas, and an oxygen-containing gas in a first zone of a flow-through reactor,
adding from 70-100% of the total amount of at least one hydrolysable or oxidizable or both hydrolyzable and oxidizable silicon compound to the mixture in a second zone of the flow-through reactor, then
optionally cooling the mixture in a third zone of the flow-through reactor,
separating off a solid from gaseous or vaporous material in the third zone of the flow-through reactor, and
optionally treating the solid with a surface modifying agent in the third zone of the flow-through reactor.
10. The process according to claim 9 , wherein an average residence time in the first zone is from 10 ms to 1 s and a temperature in the first zone is from 800 to 1300° C.
11. The process according to claim 9 , wherein an average residence time in the second zone is from 0.1 to 10 s and a temperature in the second zone is from 400 to 800° C.
12. The process according to claim 9 , wherein adding the at least one silicon compound is exclusively in the second zone.
13. The process according to claim 9 , wherein the at least one silicon compound is at least one selected from the group consisting of SiCl 4 , CH 3 SiCl 3 , (CH 3 ) 2 SiCl 2 , (CH 3 ) 3 SiCl, HSiCl 3 , (CH 3 ) 2 HSiCl and CH 3 C 2 H 5 SiCl 2 , H 4 Si, Si(OC 2 H 5 ) 4 , and Si(OCH 3 ) 4 .
14. The process according to claim 9 , further comprising introducing water or water vapor in the second zone.
15. A dispersion, comprising the particle of claim 1 .
16. A silicone rubber comprising the iron-silicon oxide particle according to claim 1 .
17. A rubber mixture, polymer preparation, adhesive composition, or molded polymer composite, comprising the particle of claim 1 .
18. A process of manufacturing a rubber mixture, polymer preparation, adhesive composition, or molded polymer composite, the process comprising manufacturing the rubber mixture, polymer preparation, adhesive composition, or molded polymer composite with the particle of claim 1 by fusion in an alternating electromagnetic field.