EP1899433A2 - Leitflüssigkeit mit magnetischen teilchen im millimeterbereich - Google Patents

Leitflüssigkeit mit magnetischen teilchen im millimeterbereich

Info

Publication number
EP1899433A2
EP1899433A2 EP06778666A EP06778666A EP1899433A2 EP 1899433 A2 EP1899433 A2 EP 1899433A2 EP 06778666 A EP06778666 A EP 06778666A EP 06778666 A EP06778666 A EP 06778666A EP 1899433 A2 EP1899433 A2 EP 1899433A2
Authority
EP
European Patent Office
Prior art keywords
magnetic
particles
alloys
conductive fluid
alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP06778666A
Other languages
English (en)
French (fr)
Inventor
Jean Chevalet
Emmanuelle Dubois
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Centre National de la Recherche Scientifique CNRS
Universite Pierre et Marie Curie
Original Assignee
Centre National de la Recherche Scientifique CNRS
Universite Pierre et Marie Curie
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Centre National de la Recherche Scientifique CNRS, Universite Pierre et Marie Curie filed Critical Centre National de la Recherche Scientifique CNRS
Publication of EP1899433A2 publication Critical patent/EP1899433A2/de
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C15/00—Cooling arrangements within the pressure vessel containing the core; Selection of specific coolants
    • G21C15/28—Selection of specific coolants ; Additions to the reactor coolants, e.g. against moderator corrosion
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/10—Liquid materials
    • C09K5/12—Molten materials, i.e. materials solid at room temperature, e.g. metals or salts
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Definitions

  • the present invention relates to a composite material consisting of particles of magnetic material and a conductive liquid.
  • heat transfer fluids in refrigeration or heating systems, in particular in heat exchangers in industrial environments such as those of nuclear power plants or solar energy converters.
  • Heat transfer fluids are generally constituted by liquid chemical compounds or mixtures of these compounds such as ethylene glycol, propylene glycol oils derived from petroleum, or silicones. Mention may also be made of mixtures of heavy polyaromatic compounds, aryl ethers, terphenyls, which are particularly resistant to high temperatures and which allow operation up to about 300 ° C. It is also known to use certain organic molten salts containing particulate additives as heat transfer fluid. Such materials can be used over a wide range of temperatures and the role of the particulate additives is to improve the thermal conductivity.
  • the flow of fluids is generally caused by mechanical systems, including moving parts, including blades and pumps. These mechanical systems undergo wear due in particular to the friction caused by the passage of the coolant. In addition, when used at temperatures above about 350 0 C, these fluids undergo excessive rapid degradation and cause problems of vapor pressure. Their use in the field of heat exchangers of high power and high temperature for example is excluded.
  • the object of the present invention is to provide a material capable of serving as a heat transfer fluid which eliminates the disadvantages of the systems of the prior art, namely the wear of mechanical parts, and which increases the maximum temperature of use.
  • the present invention relates to a composite material, a process for its preparation, and its applications.
  • the composite material according to the present invention consists of a carrier fluid B and particles of magnetic material A. It is characterized in that:
  • Material A is chosen from magnetic compounds and magnetic alloys, and is in the form of particles whose mean diameter is between 0.1 and 2 mm;
  • the support fluid B is a conductive fluid chosen from metals, metal alloys and salts which are liquid at temperatures below the Curie temperature of the material A, or from their mixtures.
  • a material according to the invention has a high electrical conductivity as well as a high thermal conductivity and, although heterogeneous, it can remain stable due to the good wetting of A by B when the densities are close.
  • the magnetic material A may be chosen from metals and magnetic metal oxides, magnetic alloys and magnetic compounds.
  • metals and metal oxides mention may be made of iron, iron oxide, cobalt, and nickel.
  • alloys mention may be made of steel, and alloys with high magnetic permeability.
  • An alloy with high magnetic permeability is an alloy having an initial permeability greater than 1000. Such alloys are described in particular in Chapter 2 of the work "Magnetic alloys and ferrites", MG Say, Ed. Dunod, Paris, 1956.
  • alloy of high permeability mention may be made in particular alloys of iron and silicon, and alloys consisting essentially of Ni and Fe and marketed under the name Mumétal® or Permalloy®.
  • amorphous magnetic alloys such as, for example, alloys of Fe, Co and Ni containing approximately 20% of B, C, Si or P, and alloys.
  • magnetic nanocrystalline such as for example Fe / Cu / Nb / Si / B alloys and Fe / Zr / B / Cu alloys.
  • the material A may consist of substantially spherical particles having a mean diameter between 0.1 and 2 mm.
  • the material A can also be in the form of two batches: a first batch consisting of substantially spherical particles having a mean dimension between 0.1 and 2 mm; a second batch of micrometric particles, whose size distribution is homogeneous, for example between 1 nm and 50 microns.
  • the particles of magnetic material may further consist of a batch of a first magnetic material A and a batch of a second magnetic material A 'selected from the group defined for A.
  • electrically conductive fluid is meant a fluid which has an electrical resistivity of less than about 1000 ohms per centimeter in the temperature range in which the electrolysis takes place.
  • the electrically conductive fluid B When the electrically conductive fluid B is a metal, it may be chosen from metals which are liquid alone or in the form of mixtures of several of them at temperatures below the Curie point of the magnetic material with which they are associated. By way of example, there can be mentioned Hg, Ga, In, Sn, As, Sb, alkali metals, and mixtures thereof.
  • the electrically conductive fluid B When the electrically conductive fluid B is a molten metal alloy, it may be chosen in particular from In / Ga / As alloys, Ga / Sn / Zn alloys, In / Bi alloys, the Wood alloy, the alloy of Newton, the Arcet alloy, the Lichtenberg alloy, and the Rosé alloy. Some of these alloys are commercially available. The composition and melting temperature of some of them are given below:
  • Arcet alloy Bi 50, Sn 25 - Pb 25 98
  • salts that may constitute the conductive fluid B include: alkylammonium nitrates in which the alkyl group comprises from 1 to 18 carbon atoms, guanidinium nitrates, imidazolium nitrates, imidazolinium nitrates alkali metal chloroaluminates which are liquid at temperatures above 150 ° C., the salts comprising a BF 4 " anion, FFf or trifluoroacetate and a cation chosen from amidinium ions
  • each R substituent independently of the other H or an alkyl radical having 1 to 8 carbon atoms said salts having conductivities up to 10 mS / cm and a high stability.
  • bis (trifluoromethylsulfonyl) imide of 1-ethyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide of 1-ethyl-3-methylimidazolium.
  • the composite materials according to the invention include in particular the materials constituted by the following: steel balls / Hg, steel balls / Ga, steel balls 1 + Fe powder / Hg, balls of steel + Fe / Ga powder.
  • Another object of the present invention is a process for producing the composite material. The method comprises introducing a precursor of the magnetic material A into an electrically conductive fluid B, and is characterized in that it is electrochemically implemented in an electrochemical cell in which:
  • the electrolyte is constituted by an ionic conductive medium containing the precursor of the material A, under particle shape with an average diameter of between 0.1 and 2 mm;
  • the precursor of the material A is a nonionic precursor in solution;
  • the cathode is constituted by a film of conductive fluid B connected to a source of potential, capable of delivering a current density between 100 nm and 3 amper / cm 2 ;
  • the anode is constituted by a non-oxidizable material under the process conditions, for example platinum or vitreous carbon;
  • the cathode is subjected to a negative potential difference with respect to the anode.
  • the electrolysis can be controlled either by current with a control of the evolution of the potential of the cathode, or in potential with respect to a reference electrode (with the aid of a servo-control device of the potentiostatic type) .
  • the potential applied to the cathode must in all cases be the most negative possible to allow the reduction of the interfacial tension between the materials A and B, but it will have to be limited not to cause other electro-chemical reactions such as the excessive release of hydrogen or the formation of amalgam, detrimental to the performance and stability of the product.
  • the anode can be placed in a compartment separated from the cathode by a porous wall.
  • the cell further comprises a reference electrode, when the electrolysis is controlled in potential.
  • the nonionic precursor in solution of the magnetic material A can be chosen from metals and metal oxides, as well as from the alloys mentioned above.
  • the precursor is introduced into the ionic conductive medium forming the electrolyte in the form of particles which are preferably substantially spherical.
  • the precursor is in the form of beads having a heterogeneous size distribution.
  • the precursor of the magnetic material is introduced in the form of two batches: one first batch consisting of substantially spherical particles having a mean size between 0.1 and 2 mm; a second batch of micrometric particles, whose size distribution is homogeneous, for example between 1 nm and 50 microns.
  • the precursor particles may also be constituted by a batch of a precursor of a first magnetic material A and by a batch of a precursor of a second magnetic material A 'chosen from the group defined for A.
  • the respective quantities of precursor of material A and of conducting fluid B are such that the final concentration of particles of magnetic material in conducting fluid B remains below the value beyond which the dispersion becomes biphasic or solid, which would result in a precipitation, taking into account the degree of solubility of A in B. The determination of this value is within the reach of the skilled person.
  • the precursor particles may be used as defined above. They can also be used after coating them with a metal having an affinity for A in the conducting fluid B.
  • the conducting fluid B used during the preparation of the composite material according to the invention is chosen from the conductive fluids defined above for the material itself.
  • the electrically conductive fluid B is made of a given metal, one or more elements can be added which can form a stable liquid phase (or a liquid amalgam when said metal is mercury) and which stabilize the dispersion of the particles A within of the conductive fluid avoiding their aggregation.
  • B is mercury
  • the presence of impurities is capable of significantly modifying the interfacial properties between the magnetic material A and the conducting fluid B, and therefore the wettability of the material A by the conducting fluid B. If the implementation of the process of the invention for a given A / B couple does not achieve a suitable result, it is recommended to check the nature and rate of impurities.
  • the method of the present invention can be implemented in particular for the preparation of a composite material having magnetic properties and electrical and thermal conduction properties from the precursors and the above electrically conductive fluids. It is particularly useful for the preparation of a composite material in which the material constituting the magnetic particles A and the material constituting the electrically conductive fluid B have little or no affinity between them, and when the magnetic material is better than weakly wettable by the electrically conductive fluid.
  • conductive ferrofluid materials containing the following elements:
  • the precursor particles of A may be introduced into the ionic conductive medium and then into the electrically conductive liquid B during electrolysis, i.e., gradually until the desired concentration is achieved in B.
  • the current density and / or the potential are modified simultaneously with the precursor introduction of A, which makes it possible, if necessary, to introduce precursor particles of A 'different from the precursor particles of A.
  • the ionic conductive medium is preferably non-oxidizing. It may consist of a solution of a non-oxidizing acid (for example HCl) or a strong base in a solvent.
  • the solvent may be water, a polar organic liquid or a molten salt.
  • Polar organic liquid can be selected from acetonitrile, acetone, dimethylformamide (DMF), dimethylsulfoxide (DMSO), propylene carbonate (PC), dimethyl carbonate, and N-methylpyrrolidone.
  • the molten salt can be selected from among those 5 . have been defined above as an electrically conductive fluid.
  • the potential source to which the cathode is connected must be capable of delivering a current current of at least one hundred mA / cm 2 of cathode.
  • the electrochemical cell When the electrochemical cell is controlled in potential, it necessarily comprises a reference electrode, and the potential difference between the cathode and said reference electrode is set in a range such that the interfacial tension between A and B is decreased to allow the wetting of the particles A by the liquid B.
  • the particles A are Fe particles and the liquid B is Hg
  • the voltage is between -1 V and -3 V relative to the reference electrode.
  • the electrochemical cell When the electrochemical cell operates in galvanostatic mode 0, that is to say when it is current-controlled, and it comprises a reference electrode, it is necessary to impose action thresholds which cause the reduction. of the current, so that the potential difference between the cathode and the reference electrode is limited to the defined domain for the case where the cell is controlled in potential.
  • the electrochemical cell When the electrochemical cell is current-controlled without a servo-control device and does not include a reference electrode, the total potential must be monitored with respect to a previously determined limit, eg using a temporary reference electrode.
  • an electrochemical cell comprising a reference electrode.
  • a magnetic field perpendicular to the plane of the cathode is applied in such a way that subtract the magnetic particles A formed from the electrolyte / cathode interface area, in order to control the kinetics of their growth during the initial phases of their formation.
  • other types of action on the material being synthesized can be obtained by superimposing pulses or alternating components on the current or the potential controlling the process, in the absence or in the presence of said perpendicular magnetic field.
  • the conductive fluid constituting the cathode is highly enriched in magnetic particles A and is the electrically conductive ferrofluid material of the invention.
  • a third object of the invention is the use of the composite material as heat transfer fluid.
  • the presence of magnetic particles makes it possible to move the material inside the tubes in which it is supposed to circulate by simple induction effect, which eliminates the need for mechanical parts subject to wear.
  • the metallic nature of this electrically conductive support fluid and its thermal conduction greater than that of the usual fluids (even doped with metal particles) promotes the transport of calories.
  • Iron powder marketed under ref. 312-31 (reduced iron for analysis) by the company Riedel-de Ha ⁇ n, consisting of spherical particles having a diameter of about 10 ⁇ m
  • the materials were prepared in an electrochemical cell which is connected to a source of potential and provided with stirring means, and in which the cathode is constituted by a layer of the electrically conductive fluid B, a platinum electrode ensures contact with the cathode, a second platinum electrode functions as anode, a calomel electrode functions as a reference electrode.
  • the volume fraction of iron in the material obtained is 0.127.
  • the saturation magnetization measured for this material is 250 kA / m.
  • the initial susceptibility to low magnetic field is 1.45.
  • the saturation magnetization measured for this material is 72 kA / m.
  • the initial susceptibility to low magnetic field is 0.42.
  • the volume fraction of magnetic material in the material obtained is of the order of 0.08.
  • the saturation magnetization of the material is 110 kA / m.
  • the initial susceptibility to low magnetic field is 3.5.

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Conductive Materials (AREA)
EP06778666A 2005-06-27 2006-06-26 Leitflüssigkeit mit magnetischen teilchen im millimeterbereich Withdrawn EP1899433A2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0506509A FR2887680A1 (fr) 2005-06-27 2005-06-27 Fluides conducteurs contenant des particules magnetiques millimetriques
PCT/FR2006/001469 WO2007000509A2 (fr) 2005-06-27 2006-06-26 Fluide conducteur contenant des particules magnetiques millimetriques

Publications (1)

Publication Number Publication Date
EP1899433A2 true EP1899433A2 (de) 2008-03-19

Family

ID=35976780

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06778666A Withdrawn EP1899433A2 (de) 2005-06-27 2006-06-26 Leitflüssigkeit mit magnetischen teilchen im millimeterbereich

Country Status (6)

Country Link
US (1) US8404140B2 (de)
EP (1) EP1899433A2 (de)
JP (1) JP4989642B2 (de)
CA (1) CA2612452A1 (de)
FR (1) FR2887680A1 (de)
WO (1) WO2007000509A2 (de)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101373387B1 (ko) 2006-09-22 2014-03-13 바스프 에스이 자기유변 제제
WO2008055523A1 (en) * 2006-11-07 2008-05-15 Stichting Dutch Polymer Institute Magnetic fluids and their use
JP5688500B2 (ja) * 2011-03-09 2015-03-25 樫原　宏 強磁性有機磁性流体
US8580886B2 (en) 2011-09-20 2013-11-12 Dow Corning Corporation Method for the preparation and use of bis (alkoxysilylorgano)-dicarboxylates
US9518072B2 (en) 2011-12-02 2016-12-13 Dow Corning Corporation Ester-functional silanes and the preparation and use thereof; and use of iminium compounds as phase transfer catalysts
EP2862912B1 (de) * 2013-05-07 2018-10-17 Institute of Modern Physics, Chinese Academy of Sciences Wärmeaustauschmedium, wärmeaustauschsystem und kernreaktoranlage

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JP3935870B2 (ja) * 2003-04-21 2007-06-27 独立行政法人 日本原子力研究開発機構 金属等のナノサイズ超微粒子を分散させた液体アルカリ金属
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Also Published As

Publication number Publication date
JP4989642B2 (ja) 2012-08-01
CA2612452A1 (fr) 2007-01-04
US8404140B2 (en) 2013-03-26
WO2007000509A3 (fr) 2007-05-31
US20090173907A1 (en) 2009-07-09
WO2007000509A2 (fr) 2007-01-04
FR2887680A1 (fr) 2006-12-29
JP2008547233A (ja) 2008-12-25

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