DE1696718A1 - Magnetic material and method of making the same - Google Patents

Magnetic material and method of making the same

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Publication number
DE1696718A1
DE1696718A1 DE19651696718 DE1696718A DE1696718A1 DE 1696718 A1 DE1696718 A1 DE 1696718A1 DE 19651696718 DE19651696718 DE 19651696718 DE 1696718 A DE1696718 A DE 1696718A DE 1696718 A1 DE1696718 A1 DE 1696718A1
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Germany
Prior art keywords
iron
magnetic material
ammonia
cation
calcium
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
DE1696718B2 (en
Inventor
Paul Hagenmuller
Joseph Portier
Gerard Villers
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Centre National de la Recherche Scientifique CNRS
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Centre National de la Recherche Scientifique CNRS
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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

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    • 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

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  • 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

Centre National de la Recherche Scientifique, Paris (France) Case: C.N.R.S. 25Center National de la Recherche Scientifique, Paris (France) Case: C.N.R.S. 25th

m Magnetisches Material und Verfahren zur Herstellung m Magnetic material and method of manufacture

desselben.same.

Gegenstand der Erfindung ist ein neues magnetisches Material, das durch eine der folgenden Formeln defieniert ist:The invention relates to a new magnetic material which is defined by one of the following formulas is:

[TO (NH)] M. η NH3 oder [TO(NH)] 2D. η NH3,[TO (NH)] M. η NH 3 or [TO (NH)] 2 D. η NH 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 trivalent iron 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.

Fr/ki - lt.11.1969 - 2 -Fri / ki - according to 11.1969 - 2 -

Unterlagen (Art. 7 § I Abs. 2 Nr. I Satt 3 des Ändarunaegee. v. +. H. Documents (Art. 7 § I, para. 2 no I saturated the third of Ändarunaegee. V. +. H.

109847/U17109847 / U17

Diese 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 are called "imidoferrites", since they can be regarded as normal ferrites in which one oxygen atom has been replaced by the group NH.

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

Die Imidoferrite gemäß der Erfindung werden in der Weise hergestellt, daß flüssiges Ammoniak auf ein Oxyhalogenid des Metalles T oder auf eine Mischung von Oxyhalogeniden des Metalles 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 made in the manner produced that liquid ammonia on an oxyhalide of the metal T or on a mixture of oxyhalides of the metal T, especially on iron oxychloride FeOCl, in the presence of the cation M or D to act is brought and if the connection thus obtained has a certain. Number of ammonia molecules it contains are the the latter in whole or in part by pumping out in a vacuum or by controlled pyrolysis at low temperature removed.

Die Erfindung soll anhand 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 NKLCompounds of the type [TO (NH ^ M. η NKL

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

Zwei Gramm Eisenoxychlorid FeOCl werden rn.it 0,3 g metallischem Lithium, das in hundert 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)Two grams of iron oxychloride FeOCl are mixed with 0.3 g of metallic Lithium dissolved in one hundred ml of carefully dried liquid ammonia made to react. The reaction, which can be recognized by the release of hydrogen, corresponds to equation (1) given below

109847/1417109847/1417

ORiGlNAL INSPECTEDORiGlNAL INSPECTED

und findet von -600C 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: [FeO(NH)] Li.NH3. Durch Pyrolyse zwischen 70 und 1200C verliert diese Verbindung ein Molekül Ammoniak, welches 15,3 % des Gewichtes darstellt, gemäß der Reaktionsgleichung (2), die weiter unten angegeben ist.and finds from -60 0 C to take. It takes about 30 minutes. After evaporation of the liquid ammonia, a powder is obtained which consists of a mixture of LiCl and a phase with magnetic properties. The latter is separated by magnetic sorting. This gives 1.5 g of a black powder which, according to chemical analysis, corresponds to the following formula: [FeO (NH)] Li.NH 3 . By pyrolysis between 70 and 120 0 C this compound loses a molecule of ammonia, which represents 15.3% of the 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 Fe3O3 und Lithium durch ein spektrophotometrxsches 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 3 O 3 and lithium were determined by a spectrophotometric method. The experimental results in percent by weight are as follows:

Fe 60 %, N 14,3 %, Li 72 %.Fe 60%, N 14.3%, Li 72%.

Diese Zusammensetzung stimmt gut mit der Formel [FeO(NH)/ Li überein. Die danach berechneten Werte sind folgende:This composition agrees well with the formula [FeO (NH) / Li match. 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:

(1) FeOCl + 2Li + 2NH3 5>[f"eO(NH)] LiNH3 + LiCl + H2 (1) FeOCl + 2Li + 2NH 3 5> [f "eO (NH)] LiNH 3 + LiCl + H 2

(2) [FeO(NH)] Li-NH3 ^eO(NH)] Li + NH3.(2) [FeO (NH)] Li-NH 3 ^ eO (NH)] Li + NH 3 .

Das magnetische Moment wurde an [FeO(NH)] Li in einem Feld von 20 000 Oersted bei Zimmertemperatur gemessen und betrug:The magnetic moment was measured on [FeO (NH)] Li in a field of 20,000 Oersted at room temperature and was:

Cf s 30 e.g.s.Cf s 30 egs

109847/1417109847/1417

Die Verbindungen [FeO(NHUNa-NH3, fFeO(NH)J K.NH3 sowie [FeO(NH)JNa und ["FeO(NHgK werden unter den gleichen Versuchsbedingenen erhalten. The compounds [FeO (NHUNa-NH 3 , fFeO (NH) J K.NH 3 and [FeO (NH) JNa and ["FeO (NHgK) are obtained under the same experimental conditions.

Verbindungen des Typs [TO(NH)I2 D. nNHg Compounds of the type [TO (NH) I 2 D. nNH g

Die Herstellung von Verbindungen dieses Typs wird durch folgendes Beispiel veranschaulicht:The production of compounds of this type is illustrated by the following example:

Kalzium wird bei -1IO0C »it Eisenoxychlorid FeOCl zur Reaktion gebracht.Calcium is in - brought one IO 0 C »it FeOCl iron oxychloride to react.

Die Umsetzung verläuft nach folgender Gleichung: 2FeOCl + 2Ca + (x+2)NH3 » [FeO(NH)]I2 Ca.XNH3 + CaCl2 + 2H2 The conversion proceeds according to the following equation: 2FeOCl + 2Ca + (x + 2) NH 3 »[FeO (NH)] I 2 Ca.XNH 3 + CaCl 2 + 2H 2

Bei der Pyrolyse unter Vakuum wird Ammoniak gemäß der folgenden Gleichung abgegeben: In pyrolysis under vacuum , ammonia is given off according to the following equation :

[FeO(NH)I2 Ca.XNH3 > [FeO(NH)] 2 Ca + XNH3.[FeO (NH) I 2 Ca. XNH 3 > [FeO (NH)] 2 Ca + XNH 3 .

Die Verbindungen [FeO(NH)J2 Mg.XNH3 und [FeO(NH)J2 Mg werden unter den gleichen Versuchsbedingenen erhalten.The compounds [FeO (NH) I 2 Mg. XNH 3 and [FeO (NH) I 2 Mg are obtained under the same experimental conditions.

Die Erfindung ist jedoch nicht auf die Ausführungsbeispiele beschränkt.The invention is not limited to the embodiments.

Anlage:System:

4 Patentansprüche4 claims

1Ü9847/U171Ü9847 / U17

Claims (3)

PatentansprücheClaims 1.) Magnetisches Material, gekennzeichnet durch eine Zusammensetzung gemäß der Formel1.) Magnetic material, characterized by a composition according to the formula [TO(NH)]M. η NH3 oder
[TO(NH)I2D. η NH3,[TO (NH)] M. η NH 3 or
[TO (NH) I 2 D. η NH 3 , bei der T mindestens teilweise dreiwertiges Eisen und der eventuelle Rest andere dreiwertige Kationen, wie Aluminium und Chrom, bedeutet,at T at least partially trivalent iron and the remainder, if any, other trivalent cations, such as aluminum and chrome, means M ein einwertiges Kation von Lithium, Natrium, Kalzium, Kupfer, Silber oder Thallium bedeutet,M means a monovalent cation of lithium, sodium, calcium, copper, silver or thallium, D ein zweiwertiges Kation von Beryllium, Magnesium, Kalzium, Strontium, Barium, Kupfer, Zink, Kadmium, Quecksilber, Mangan, Eisen, Kobalt oder Nickel bedeutet,D a divalent cation of beryllium, magnesium, calcium, strontium, barium, copper, zinc, cadmium, mercury, Means manganese, iron, cobalt or nickel, 0, N und H ihre übliche Bedeutung haben und0, N and H have their usual meanings and η eine beliebige Zahl einschließlich Null bedeutet.η means any number including zero. 2.) Verfahren zur Herstellung von magnetischem Material nach Anspruch 1, dadurch gekennzeichnet, daß ein Oxyhalogenid des Metalles T oder eine Mischung von Oxyhalogeniden der Metalle T auf das Kation M oder D in flüssigem Ammoniak zur Einwirkung gebracht wird.2.) Process for the production of magnetic material according to Claim 1, characterized in that an oxyhalide of the metal T or a mixture of oxyhalides of Metals T is brought into action on the cation M or D in liquid ammonia. 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, for the partial or complete removal of the Ammonia is pumped down under vacuum or subjected to controlled pyrolysis at low temperature. U.) Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß flüssiges Ammoniak auf Eisenoxychlorid FeOCl zur Einwirkung gebracht wird.U.) Method according to claim 1 and 2, characterized in that that liquid ammonia on iron oxychloride FeOCl for Action is brought. Fr/ki - 14.11.1969Fri / ki - 11/14/1969 109847/U17
Neue Unterlasen (Art7iiAte.2Nr.iv 109847 / U17
New Unterlasen (Art7iiAte.2Nr.i v
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 true DE1696718A1 (en) 1971-11-18
DE1696718B2 DE1696718B2 (en) 1975-11-27

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Family Applications (1)

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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)

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* 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
DE1696718B2 (en) 1975-11-27
FR1403880A (en) 1965-06-25
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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