DE1696718B2 - Magnetic material and method of making the same - Google Patents

Magnetic material and method of making the same

Info

Publication number
DE1696718B2
DE1696718B2 DE19651696718 DE1696718A DE1696718B2 DE 1696718 B2 DE1696718 B2 DE 1696718B2 DE 19651696718 DE19651696718 DE 19651696718 DE 1696718 A DE1696718 A DE 1696718A DE 1696718 B2 DE1696718 B2 DE 1696718B2
Authority
DE
Germany
Prior art keywords
magnetic material
ammonia
feo
cation
iron
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.)
Granted
Application number
DE19651696718
Other languages
German (de)
Other versions
DE1696718A1 (en
Inventor
Paul Merignac Gironde Hagenmuller
Joseph Talence Portier
Gerard Bellevue Seine-Et-Oise Villers
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
Original Assignee
Centre National de la Recherche Scientifique CNRS
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 filed Critical Centre National de la Recherche Scientifique CNRS
Publication of DE1696718A1 publication Critical patent/DE1696718A1/en
Publication of DE1696718B2 publication Critical patent/DE1696718B2/en
Granted legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2683—Other ferrites containing alkaline earth metals or lead
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
    • C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
    • C01B21/0923—Metal imides or amides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2616—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing lithium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2625—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing magnesium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Compounds Of Iron (AREA)
  • Soft Magnetic Materials (AREA)
  • Catalysts (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

Gegeiistand der Erfindung ist ein neues magnetitches Material, das durch eine der folgenden Formeln definiert ist:Object of the invention is a new magnetitches Material defined by one of the following formulas:

[TO(NH)]M-TiNH3
[TO(NH)]2D-/1NH3 [TO (NH)] M-TiNH 3
[TO (NH)] 2 D- / 1NH 3

in denen T mindestens teilweise dreiwertiges Eisen bedeutet und der eventuelle Rest durch ein anderes dreiwertiges Kation der Gruppe Aluminium und Chrom gebildet wird.in which T is at least partially trivalent iron and the remainder, if any, is another trivalent cation of the group aluminum and chromium is formed.

M ist ein einwertiges Kation aus der Gruppe Lithium, Natrium, Kalium, Kupfer, Silber und Thallium.M is a monovalent cation from the group consisting of lithium, sodium, potassium, copper, silver and Thallium.

D ist ein zweiwertiges Kation aus der Gruppe Beryllium, Magnesium, Kalzium, Strontium, Barium, Kupfer, Zink. Kadmium, Quecksilber, Mangan, Eisen, Kobalt und Nickel.D is a divalent cation from the group beryllium, magnesium, calcium, strontium, barium, Copper, zinc. Cadmium, mercury, manganese, iron, cobalt and nickel.

C, N und H haben ihre übliche Bedeutung und η bedeutet jede Zahl einschließlich Null.C, N and H have their usual meanings and η means any number including zero.

Dies" neuen Zusammensetzungen werden »Imidoferrite: < genannt, da sie als normale Ferrite betrachtet werden können, in denen ein Sauerstoffatom durch die Gruppe NH ersetzt ist.These "new compositions will be» imido ferrites: <because they can be regarded as normal ferrites in which an oxygen atom is replaced by the group NH.

Mindestens einige dieser Imidofemte zeigen eine starke spontane Magnetisierung, welche es erlaubt, sie für bestimmte technische Anwendungen an Stelle der üblichen Ferrite zu verwenden.At least some of these imidofemts show one strong spontaneous magnetization, which allows them to be used for certain technical applications the usual ferrites to be used.

Die Imidoferrite gemäß der Erfindung werden in der Weise hergestellt, daß flüssiges Ammoniak auf ein Oxyhalogenid des Metalls T oder auf eine Miseren» von Oxyhalogeniden des Metalls T, insbesondere auf Eisenoxychlorid FeOCl, in der Gegenwart des Kations M oder D zur Einwirkung gebracht wird und wenn die so erhaltene Verbindung eine gewisse Anzahl von Ammoniakmolekülen enthält, werden die letzteren ganz oder teilweise durch Abpumpen im Vakuum oder durch gesteuerte Pyrolyse bei niedriger Temperatur entfernt.The imidoferrites according to the invention are produced in such a way that liquid ammonia an oxyhalide of the metal T or a misery » of oxyhalides of the metal T, in particular on iron oxychloride FeOCl, in the presence of the cation M or D is brought into action and if the compound thus obtained has a certain Number of ammonia molecules, the latter are wholly or partly by pumping out in the Removed vacuum or by controlled pyrolysis at low temperature.

Die Erfindung soll an Hand von Ausführungsbeispielen näher erläutert werden.The invention is to be explained in more detail on the basis of exemplary embodiments.

Verbindungen des Typs [TO(NH)]M · η NH1 Compounds of the type [TO (NH)] M · η NH 1

Das erste Beispiel bezieht sich auf die Herstellung des Lithium-Imidofcrrits [FeO(NH)]Li.The first example relates to the production of the lithium imidofrite [FeO (NH)] Li.

Zwei Gramm Eisenoxychlorid FeOCl werden mit 0,3 g metallischem Lithium, das in 100 ml von sorgfältig getrocknetem flüssigem Ammoniak gelöst ist, zur Reaktion gebracht. Die Reaktion, welche durch die Abgabe von Wasserstoff erkennbar ist, entspricht der unten angegebenen Gleichung (1) und findet von -60° C an statt. Sie dauert etwa 30 Minuten. Nach Verdampfen des flüssigen Ammoniaks wird ein Pulver erhalten, das aus einer Mischung von LiCl und einer Phase mit magnetischen Eigenschaften besteht. Die letztere wird durch magnetisches Aussortieren abgetrennt. Es werden auf diese Weise 1,5 g eines schwarzen Pulvers erhalten, welches nach der chemischen Analyse der folgenden Formel entspricht:Two grams of iron oxychloride FeOCl are mixed with 0.3 g of metallic lithium, which in 100 ml of carefully dried liquid ammonia is dissolved, brought to reaction. The reaction which by the release of hydrogen is recognizable, corresponds to equation (1) given below and takes place from -60 ° C instead. It takes about 30 minutes. After evaporation of the liquid ammonia it becomes a powder obtained, which consists of a mixture of LiCl and a phase with magnetic properties. The latter is separated by magnetic sorting. In this way 1.5 g of one are obtained black powder obtained which, according to chemical analysis, corresponds to the following formula:

[FeO(NH)]Li · NH3 [FeO (NH)] Li • NH 3

Durch Pyrolyse zwischen 70 und 120° C verliert diese Verbindung ein Molekül Ammoniak, welches 15,3% des Gewichtes darstellt, gemäß der Reaktionsgleichung (2), die weiter unten angegeben ist.Loses between 70 and 120 ° C through pyrolysis this compound is a molecule of ammonia, which represents 15.3% by weight, according to the reaction equation (2), which is given below.

In der so erhaltenen Verbindung wurde Stickstoff in Form von NH3 bestimmt, Eisen in Form von Fe0O1 und Lithium durch ein spektrophotometrisches Verfahren. Die experimentellen Ergebnisse in Gewichtsprozent sind folgende:In the compound thus obtained, nitrogen in the form of NH 3 , iron in the form of Fe 0 O 1 and lithium were determined by a spectrophotometric method. The experimental results in percent by weight are as follows:

40 Fe 6O°/o, 40 Fe 60 ° / o,

N 14,3%, Li 72%.N 14.3%, Li 72%.

55 Diese Zusammensetzung stimmt gut mit der Formel [FeO(NH)]Li überein. Die danach berechneten Werte sind folgende: 55 This composition agrees well with the formula [FeO (NH)] Li. The calculated values are as follows:

Fe 59,54%, N 14,93%, Li 7,40%.Fe 59.54%, N 14.93%, Li 7.40%.

Die bei der Herstellung ablaufenden Reaktionen sind folgende:The reactions that take place during production are as follows:

FeOCl + 2 Li + 2 NH3 -> [FeO(NH)]LiNH3 + LiCl + H2 (1)FeOCl + 2 Li + 2 NH 3 -> [FeO (NH)] LiNH 3 + LiCl + H 2 (1)

[FeO(NH)]Li · NH3 -> [FeO(NH)]Li + NH3 (2)[FeO (NH)] Li · NH 3 -> [FeO (NH)] Li + NH 3 (2)

3 43 4

Das magnetische Moment wurde an [FeO(NH)]Li [FeO(NH)]K werden unter den gleichen Versuchsin einem Feld von 20000 Oersted bei Zimmertempe- bedingungen erhalten,
ratur gemessen und betrug: Verbindungen des Typs [TO(NH)]2D · η NK3 The magnetic moment was obtained on [FeO (NH)] Li [FeO (NH)] K under the same experiment in a field of 20,000 Oersted at room temperature conditions,
temperature and was: compounds of the type [TO (NH)] 2 D · η NK 3

a = 30 c.g.s. 5 Die Herstellung von Verbindungen dieses Typs a = 30 cgs 5 The preparation of compounds of this type

wird durch folgendes Beispiel veranschaulicht:is illustrated by the following example:

Die Verbindungen [FeO(NH)]Na-NH3, Kalzium wird bei -4O0C mit EisenoxydchloridThe compounds [FeO (NH)] Na-NH 3 , calcium is at -4O 0 C with iron oxychloride

[FeO(NH)]K · NH3 sowie [FeO(NH)]Na und FeOCl zur Reaktion gebracht.[FeO (NH)] K · NH 3 as well as [FeO (NH)] Na and FeOCl reacted.

Die Umsetzung verläuft nach folgender Gleichung:The implementation proceeds according to the following equation:

2 FeOCl + 2 Ca -; (x + 2)NH3 -> [FeO(NH)],Ca ■ χ NH3 + CaCl2 + 2 H,2 FeOCl + 2 Ca -; (x + 2) NH 3 -> [FeO (NH)], Ca ■ χ NH 3 + CaCl 2 + 2 H,

Bei der Pyrolyse unter Vakuum wird Ammoniak gemäß der folgenden Gleichung abgegeben:
[FeO(NH)J2Ca ■ χ NH3 -> [FeO(NH)J2Ca + χNH3 In pyrolysis under vacuum, ammonia is given off according to the following equation:
[FeO (NH) J 2 Ca ■ χ NH 3 -> [FeO (NH) J 2 Ca + χ NH 3

Die Verbindungen [FeO(NH)]2Mg·.χNH3 und Die Erfindung ist jedoch nicht auf die Ausfiih-The compounds [FeO (NH)] 2 Mg ·. χ NH 3 and The invention is not limited to the execution

[FeO(NH)]2Mg werden unter den gleichen Ver- rungsbeispiele beschränkt.
Suchsbedingungen erhalten.[FeO (NH)] 2 Mg are restricted under the same conversion examples.
Get search conditions.

Claims (4)

Patentansprüche:Patent claims: 1. Magnetisches Material, gekennzeichnet durch eine Zusammensetzung gemäß der b Formel1. Magnetic material, characterized by a composition according to b formula [TO(NH)]M-TjNH3
oder[TO (NH)] M-TjNH 3
or [TO(NH)]2D · η NH3 [TO (NH)] 2 D · η NH 3 1010 bei der T mindestens teilweise dreiwertiges Eisen und der eventuelle Rest andere dreiwertige Kationen, wie Aluminium und Chrom, bedeutet, M ein einwertiges Kation von Lithium, Natrium, Kalzium, Kupfer, Silber oder Thallium bedeutet, D ein zweiwertiges Kation von Berryllium, Magnesium, Kalzium, Strontium, Barium, Kupfer, Zink, Kadmium, Quecksilber, Mangan, Eisen, Kobalt oder Nickel bedeutet, O, N und H ihre übliche Bedeutung haben und η eine beliebige Zahl einschließlich Null bedeutet.where T is at least partially trivalent iron and the remainder is other trivalent cations, such as aluminum and chromium, M is a monovalent cation of lithium, sodium, calcium, copper, silver or thallium, D is a divalent cation of berryllium, magnesium, calcium , Strontium, barium, copper, zinc, cadmium, mercury, manganese, iron, cobalt or nickel means, O, N and H have their usual meanings and η means any number including zero. 2. Verfahren zur Herstellung von magnetischem Material nach Anspruch 1, dadurch gekennzeichnet, daß ein Oxyhalogenid des Metalls T oder eine Mischung von Oxyhalogeniden der Metalle T auf das Kation M oder D in flüssigem Ammoniak zur Einwirkung gebracht wird.2. A method for producing magnetic material according to claim 1, characterized in that that an oxyhalide of the metal T or a mixture of oxyhalides of the metals T on the cation M or D in liquid Ammonia is brought into action. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die erhaltene Verbindung, wenn sie Ammoniakmoleküle enthält, zur teilweisen oder vollständigen Entfernung des Ammoniaks dem Abpumpen im Vakuum oder einer gesteuerten Pyrolyse bei niedriger Temperatur unterworfen wird.3. The method according to claim 2, characterized in that the compound obtained, if it contains ammonia molecules, to partially or completely remove the ammonia is subjected to pumping in a vacuum or a controlled pyrolysis at low temperature. 4. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß flüssiges Ammoniak auf Eiscnoxychlorid FeOCl zur Einwirkung gebracht wird.4. The method according to claim 1 and 2, characterized in that liquid ammonia Eiscnoxychlorid FeOCl is brought into action.
DE19651696718 1964-05-15 1965-05-14 Magnetic material and method of making the same Granted DE1696718B2 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR974790A FR1403880A (en) 1964-05-15 1964-05-15 New mineral compounds, in particular for magnetic applications, and their manufacturing process

Publications (2)

Publication Number Publication Date
DE1696718A1 DE1696718A1 (en) 1971-11-18
DE1696718B2 true DE1696718B2 (en) 1975-11-27

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ID=8830218

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19651696718 Granted DE1696718B2 (en) 1964-05-15 1965-05-14 Magnetic material and method of making the same

Country Status (9)

Country Link
AT (1) AT280625B (en)
BE (1) BE663913A (en)
CH (1) CH471042A (en)
DE (1) DE1696718B2 (en)
ES (1) ES312975A1 (en)
FR (1) FR1403880A (en)
GB (1) GB1035594A (en)
NL (1) NL6506159A (en)
SE (1) SE302492B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110459377A (en) * 2018-05-07 2019-11-15 中国科学院物理研究所 A kind of ferromagnetic material and preparation method thereof with huge Negative magnetoresistance effect

Also Published As

Publication number Publication date
SE302492B (en) 1968-07-22
ES312975A1 (en) 1965-12-16
FR1403880A (en) 1965-06-25
DE1696718A1 (en) 1971-11-18
GB1035594A (en) 1966-07-13
CH471042A (en) 1969-04-15
BE663913A (en) 1965-11-16
NL6506159A (en) 1965-11-16
AT280625B (en) 1970-04-27

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C3 Grant after two publication steps (3rd publication)
E77 Valid patent as to the heymanns-index 1977
8339 Ceased/non-payment of the annual fee