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Method for Manufacturing Ferrofluid s\ — Illl INI II III II I III I III II II I II OJII Eur°Pean Patent Office <*S Office europeen des brevets (11) EP 0 880 149 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) int. CI.6: H01F1/44 25.11.1998 Bulletin 1998/48 (21) Application number: 98102781.6 (22) Date of filing: 18.02.1998 (84) Designated Contracting States: (72) Inventors: AT BE CH DE DK ES Fl FR GB GR IE IT LI LU MC • Raj, Kuldip NL PT SE Merrimack, New Hampshire 03054 (US) Designated Extension States: • Aziz, Lutful M. AL LT LV MK RO SI Nashua, New Hampshire 03060 (US) (30) Priority: 21.02.1997 US 37416 P (74) Representative: 10.02.1998 US 21228 Kindermann, Manfred Patentanwalt, (71) Applicant: Sperberweg 29 Ferrofluidics Corporation 71032 Boblingen (DE) Nashua New Hampshire 03061 (US) (54) Method for manufacturing ferrof luid (57) A ferrofluid manufacturing process applies energy to a nonmagnetic <x-Fe203 starting material to render it magnetic and suitable for use in a ferrofluid. The material is placed, together with a solvent and a surfactant, in a commercial attrition mill where the mill action converts the non-magnetic particles to magnetic particles. In order to eliminate a solvent replacement step which is necessary with oil carrier liquids, water is used as the grinding solvent and as the ferrofluid carrier liquid. The resulting water-based ferrofluid has a high saturation magnetization, low viscosity and good colloi- dal stability. Using the inventive method, a large volume of fluid can inexpensively be synthesized in a short time. <7> O CO CO o Q_ LU Printed by Xerox (UK) Business Services 2.16.6/3.4 1 EP 0 880 149 A1 2 Description ids include sealing, damping, heat transfer, noise con- trol, material separation, sensing and parts inspection. FIELD OF THE INVENTION They are used in such diverse products as exclusion seals, loudspeakers and stepper motors. The industries This invention relates to processes for manufactur- s in which ferrofluid-based products are typically used ing ferrofluid in substantially larger volumes and in less are: the semiconductor, computer, aerospace, oil pros- time than is possible with existing techniques. pecting and mining industries. Known manufacturing processes for producing fer- BACKGROUND OF THE INVENTION rofluids characteristically begin by producing suitably- 11 sized particles of a ferrous material, such as Fe304 Ferrofluids are colloidal systems containing mag- (magnetite). Magnetite particles in a subdomain size netic particles, typically having a diameter of the order (e.g., about 10 nm) necessary for use in a ferrofluid, are of 10 nm, suspended in a liquid carrier. The difference not commercially available. Consequently, two methods between ferrofluids and other well-known colloids is that are used to produce suitably sized particles: ball mill ferrofluids specifically utilize particles which possess 15n grinding and chemical precipitation. These methods are magnetic properties, whereas other colloids are com- described in detail in a book entitled prised of non-magnetic particles. Commercial ferroflu- Ferrohydrodynamics by R.E. Rosensweig; Cambridge ids are generally comprised of magnetite or mixed University Press and a book entitled Magnetic Fluid ferrite particles, although it is possible to use particles of Handbook and Applications Handbook, editor B. Berko- other magnetic materials, such as iron, cobalt, nickel, 202t voski, Begell House, Inc., New York (1996). chromium dioxide, iron nitride or magnetic alloys of A typical ball mill grinding process starts with com- these materials. In general, the ferrofluid is colloidally mercially-available magnetic powder, such as magnetite stable and has a relatively low viscosity. powder, in which the particles are of "micron size", e.g. In order to form a stable colloid, the particle size about 0.15 to 0.3 microns (i.e. about 150 nm to 300 nm). should be in the range of 10 nm. In practice, the parti- 252t The commercially-available magnetite particles are cles are generally spherical in shape and are small then ground to reduce their size about 90%, to about 1 0 enough to form a single magnetic domain representing nm. A typical ball milling process is described in the U.S. a tiny permanent magnet with an associated north and Patent No. 3,917,538. In this process, proper amounts a south pole. The particles are further coated with lay- of magnetite powder, surfactant and a solvent are ers of surfactant to prevent agglomeration caused by 303< placed in a stainless steel milling jar about 40% filled magnetic and Van der Waals attractive forces. It is also with grinding media, such as 1/4" carbon steel balls. For possible to form a stable colloid by using either positive grinding to be effective, the viscosity of the solvent or negative electrical charges to keep the particles sep- should be low. In a water-based ferrofluid, the water car- arated; these formulations are referred to as "ionic fer- rier is of low viscosity and consequently, it can be used rofluids". The surfactant used in each type of ferrofluid is 353i as the solvent in the grinding process. In oil-based fer- specific to the carrier because the surfactant must be rofluid, the carrier liquid often has a relatively high vis- chemically compatible with the carrier. The particles cosity. Consequently, a low molecular weigh solvent is may be coated either with a single or double surfactant often added to the oil carrier during the grinding process layers and may be either cationic, anionic or non-ionic in to reduce the viscosity. This solvent is subsequently nature. 404t removed by evaporation to increase the saturation mag- A typical ferrofluid may consist of the following vol- netization in the final ferrofluid. ume fractions: 4% particles, 8% surfactant and 88% liq- The rolling action of the mill causes the media to uid carrier. Ferrofluids are characterized by the liquid impact repeatedly the coarse magnetite breaking it into carrier in which the particles are suspended because it subdomain size particles and coating some of the parti- is the dominant component. For example, a water- 454t cles at the same time with the surfactant. Because the based ferrofluid is a stable suspension of magnetic par- milling media generate a relatively low shear energy, a ticles in water, whereas an oil-based ferrofluid is a sta- conventional ball milling operation takes anywhere from ble suspension of magnetic particles in an oil (such as a two to six weeks to complete and the dispersion quality hydrocarbon, an ester, a fluorocarbon, a silicone oil or is poor. The colloid formed by this process generally polyphenyl ether, etc.) The physical properties of a fer- 50st includes uncoated particles and large aggregates and rofluid are also based on the selection of the liquid car- thus requires a subsequent refinement in which unde- rier since it is the majority component. In addition, as sirable particles and aggregates are removed. mentioned above, the surfactants for water- and oil- Moreover, the finished product often has a high vis- based ferrofluids are different. cosity due to the presence of small particles produced Magnetic colloids can be viewed as "liquid mag- st during the grinding process. These small particles are nets" which can be manipulated and positioned with a further known to degrade the thermal stability of the magnetic field to provide sealing and increase heat fluid. It is also believed that the process may only transfer rates. The commercial applications of ferroflu- reduce large aggregates of useful small particles which 2 3 EP 0 880 149 A1 4 are initially present in commercial magnetite powder. suitable for use in a ferrofluid. The yield is poor, preparation times are long and the In accordance with one embodiment, the nonmag- associated costs are high so that the ball milling method netic starting material is <x-Fe203 which is often is generally not considered to be suitable for a large referred to in the literature as red iron oxide. This mate- scale production of commercial ferrofluids. 5 rial is commercially available in particulate size of the Magnetite particles can also be produced by chem- order of 10 nm and, thereby, requires little or no grinding ical precipitation processes. Generally, in such proc- for the purpose of reducing its particle size. The mate- esses, magnetite particles are produced by mixing rial is placed, together with a solvent and a surfactant, in ferrous and ferric salt solutions in the presence of an a commercial attrition mill where the mill action converts alkaline medium. The resultant particles are then 10 the non-magnetic particles to magnetic particles. coated with surfactant. Both water-based and oil-based In accordance with another aspect of the invention, ferrofluids can be produced by means of this technique. water is used as the grinding solvent and as the fer- For example, U.S. Patent No. 5,240,626 discloses the rofluid carrier liquid. This eliminates the solvent replace- synthesis of a water-based ferrofluid in which nanosize ment step which is necessary with oil carriers. The magnetite particles are coated with a single carboxyl- 15 resulting water-based ferrofluid has a high saturation functional polymer surfactant. Two separate surfactant magnetization, low viscosity and good colloidal stability. coatings are used for magnetite particles in aqueous Using the inventive method, a large volume of fluid can phase in U.S. Patent No. 4,094,804. Lignosulphonate, a inexpensively be synthesized in a short time. A scale up byproduct of wood pulping, was used to prepare an to a very high production levels can be achieved easily. inexpensive water-based colloid by chemically precipi- 20 tating magnetite microcrystals as disclosed in U.S. Pat- BRIEF DESCRIPTION OF THE DRAWINGS ent No.
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