High magnetization aqueous ferrofluids and processes for preparation and use thereof

• US 5,667,716 A
• Filed: 07/01/1996
• Issued: 09/16/1997
• Est. Priority Date: 07/01/1996
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Ziolo, Ronald F., Kroll, Elizabeth C., Pieczynski, Rachel
• Primary Examiner(s): KOSLOW, CAROL M
• Application Number:
  US08/674,306
• Time in Patent Office: 442 Days
• Field of Search: 252/62.52, 252/62.54
• US Class Current: 252/62.52
• CPC Class Codes: B82Y 25/00 Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
• CPC Class Codes: H01F 1/0054 Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
• CPC Class Codes: H01F 1/0063 in a non-magnetic matrix, e.g. granular solids granular films H01F10/007
• CPC Class Codes: H01F 1/445 the magnetic component being a compound, e.g. Fe3O4 H01F1/447 takes precedence

Abstract

A ferrofluid comprising an aqueous suspension of an unsilanated or silanated nanocomposite comprised of Fe₂ O₃ nanoparticles and an ionic exchange resin, wherein the ferrofluid has a high magnetization moment of about 20 to about 40 emu/gram.

Claims

1. A process for the preparation of a high magnetization aqueous ferrofluid composition comprising:

providing a low optical density magnetic composition comprising a nanocomposite of particles comprising Fe₂ O₃ nanoparticles and an ionic exchange resin;

milling the low optical density magnetic composition;

adding liquid vehicle to the composition and thereafter milling the resulting mixture to form a colloidal suspension;

treating the colloidal suspension to form a supernatant and a residue, and thereafter separating the supernatant from the residue; and

exposing the residue to a magnetic field to generate a highly magnetic suspended component and a non- and low magnetic sludge components, wherein the highly magnetic component is an aqueous ferrofluid composition with a high magnetization moment of about 20 to about 40 emu/gram.

2. A process according to claim 1 further comprising treating the resulting aqueous ferrofluid composition with a reactive organosilane compound to form a silanated aqueous ferrofluid composition having a viscosity of from about 10^-3 to about 10^- Pa×

sec at about 25°

C., and wherein the surfaces of the magnetic nanocomposite particles of the ferrofluid are coated with a covalently bonded organosilane compound.

3. A process according to claim 2 wherein the reactive organosilane compound is selected from the group consisting of mono-, di-, and tri-halo substituted silane compounds containing substitutents independently selected from the group consisting of alkyl groups with from 1 to about 20 carbon atoms, aryl, and alkylaryl groups, with from 6 to about 25 carbon atoms.

4. A process according to claim 3 wherein the reactive organosilane compound is selected in an amount of from about 0.01 to about 2 weight percent based on the weight percent of the solids content of the aqueous ferrofluid.

5. A process according to claim 2 wherein the resulting aqueous silanated ferrofluid composition has a magnetization moment of about 30 to about 38 emu/gram.

6. A process according to claim 1 wherein the resulting aqueous ferrofluid composition has a magnetization moment of at least 34 emu/gram.

7. A high magnetization aqueous ferrofluid composition prepared by the process of claim 1.

8. A high magnetization silanated aqueous ferrofluid composition prepared by the process of claim 2.

9. A ferrofluid comprising an aqueous suspension of a nanocomposite comprised of Fe₂ O₃ nanoparticles and an ionic exchange resin, wherein the ferrofluid has a high magnetization moment of about 20 to about 40 emu/gram.

10. A ferrofluid according to claim 9 wherein the ferrofluid has a high spiking or spicule forming property wherein the spicules or spikes are from about 1.0 to about 20 millimeters in height, wherein the spikes have a high aspect ratio of about 1:

25, and a spicule resolution of about 1.0 millimeter at half peak height measured at a magnetic field of from about 200 to about 10,000 Gauss.

11. A ferrofluid according to claim 9 wherein the Fe₂ O₃ nanoparticles are present in an amount of from about 20 to about 50 weight percent, and the ionic exchange resin is present in an amount of from about 80 to about 50 weight percent, and an aqueous phase is present in an amount of about 50 to about 90 weight percent based on the total weight of the ferrofluid.

12. A ferrofluid according to claim 11 wherein the aqueous suspension comprises from about 50 to about 90 weight percent water or a mixture of water and a water miscible solvent, and from about 10 to about 50 weight percent solids.

13. A ferrofluid according to claim 12 wherein the fluid is stable over a pH range of about 5 to about 10.

14. A ferrofluid according to claim 9 wherein the Fe₂ O₃ nanoparticles have a volume average diameter of about 1 to about 10 nanometers.

15. A ferrofluid according to claim 9 wherein the aqueous suspension has a viscosity is from about 10^-3 to about 10^-1 Pa×

sec at about 25°

C.

16. A ferrofluid comprising an aqueous suspension of a silanated nanocomposite comprised of particles which are altered by treatment with a silanating agent comprised of the product of mixing a silane compound with nanoparticles of Fe₂ O₃ and an ionic exchange resin, wherein the silanated ferrofluid has a high magnetization moment of about 20 to about 40 emu/gram.

17. A ferrofluid according to claim 16 wherein the ferrofluid has a high spiking or spicule forming property wherein the spicules or spikes are from about 1.0 to about 20 millimeters in height, wherein the spikes have a high aspect ratio of about 1:

25, and a spicule resolution of about 1.0 millimeter at half peak height measured at a magnetic field of from about 200 to about 10,000 Gauss.

18. A ferrofluid according to claim 16 wherein the Fe₂ O₃ nanoparticles are present in an amount of from about 20 to about 50 weight percent, and the ionic exchange resin is present in an amount of from about 80 to about 50 weight percent, and an aqueous phase is present in an amount of about 50 to about 90 weight percent based on the total weight of the ferrofluid.

19. A ferrofluid according to claim 17 wherein the aqueous phase comprises from about 50 to about 90 weight percent water or a mixture of water and a water miscible solvent, and from about 10 to about 50 weight percent solids.

20. A ferrofluid according to claim 19 wherein the fluid is stable over a pH range of about 5 to about 10.

21. A ferrofluid according to claim 16 wherein the Fe₂ O₃ nanoparticles have a volume average diameter of about 1 to about 10 nanometers.

22. A ferrofluid according to claim 16 wherein the aqueous suspension has a viscosity greater than or equal to the viscosity of water at about 25°

C.

23. A ferrofluid according to claim 16 wherein the fluid has a shelf life of from 1 to about 36 months.