EP0469980B1 - Process for manufacturing grain non oriented magnetic steel sheet and sheet obtained thereby - Google Patents

Process for manufacturing grain non oriented magnetic steel sheet and sheet obtained thereby Download PDF

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Publication number
EP0469980B1
EP0469980B1 EP91402117A EP91402117A EP0469980B1 EP 0469980 B1 EP0469980 B1 EP 0469980B1 EP 91402117 A EP91402117 A EP 91402117A EP 91402117 A EP91402117 A EP 91402117A EP 0469980 B1 EP0469980 B1 EP 0469980B1
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Prior art keywords
tesla
sheet
process according
heat treatment
temperature
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German (de)
French (fr)
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EP0469980A1 (en
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André Bertoni
Jean-Luc Laverny
Jean Verdun
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USINOR SA
Sollac SA
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USINOR Sacilor SA
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1222Hot rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1261Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest following hot rolling

Definitions

  • the present invention relates to a method of manufacturing a sheet of magnetic steel with non-oriented grain called "fully process” and the sheet obtained by this process.
  • Such a method is known and commonly used in the field of making magnetic sheets with non-oriented grains.
  • Magnetic sheets known as non-oriented grain, that is to say having isotropic magnetic properties are more particularly intended for the construction of electromagnetic devices in which the magnetic flux generated by the electrical windings is not constant, such as for example in rotating machines.
  • Some transformers used in the household appliance sector use this type of quality for economic reasons.
  • These electromagnetic devices consist of cut and assembled sheets.
  • the latter have a degree of efficiency which is evaluated according to two parameters which are the level of induction on the one hand, and the specific total losses, on the other hand.
  • the induction is limited by the saturation magnetization of the sheets and this magnetization is higher the higher the material is rich in iron.
  • Vacuum processing improves the cleanliness and purity of the steel and thus reduces losses by hysteresis.
  • Non-oriented grain sheets made from steel with a silicon content of about 3% currently have the best magnetic loss characteristics and a lower saturation magnetization than magnetic sheets whose steel contains little or no silicon.
  • magnetic sheets with non-oriented grains are used, made with a steel containing, in its composition, only one very low silicon content, that is to say a content of less than 0.5%.
  • Document EP-A-0434641 thus discloses a composition containing 0.2 to 2% of silicon but also 0.2 to 0.5% of aluminum.
  • the so-called oriented grain sheets have a very high proportion of grains having an orientation (110). [001]. These sheets have excellent magnetic properties in the direction of rolling. They are anisotropic, that is to say that their properties depend on the direction of rolling. Thus, for example, the losses of a magnetic sheet of common composition, 0.35 mm thick, are three times higher in the direction perpendicular to the direction of rolling than in the direction of rolling.
  • Sheets with anisotropic magnetic properties therefore have the disadvantage that they can only be used for applications in which the magnetic field lines correspond to the direction of rolling. It is therefore a question of using them for static machines such as transformers.
  • the initial annealing operation after hot rolling has the function of influencing the state of the precipitates, for example MnS and / or AlN with respect to the microstructure of the sheets so as to promote the further development of the growth of oriented grains to form a GOSS texture.
  • the object of the invention is to improve the magnetic characteristics of non-oriented grain sheets made from steel containing very little silicon, that is to say to reduce the magnetic losses and to increase the magnetization under a determined magnetic field.
  • This process contributes to an improvement in the magnetic qualities, that is to say a reduction in the specific total losses and also an increase in the magnetization.
  • the steel is produced under vacuum and continuously cast in the form of slabs.
  • the sheet is produced during the hot rolling operation after rolling with slabs using a band train.
  • Table I groups together the values of the magnetic characteristics obtained in a series of tests for variation of the conditions of the heat treatment prior to cold rolling.
  • the tests were carried out by varying the temperature of the treatment from 700 ° C. to 1100 ° C., the temperature holding times being variable from 1 to 5 minutes.
  • results of the tests show, by comparison with the characteristics of a sample which has not undergone treatment, that the preliminary treatment makes it possible to increase, on the one hand the inductions of about 5% and on the other hand to reduce the losses about 12%.
  • Table II groups together, for two thicknesses of magnetic sheets, the loss characteristics in W / Kg at 50 Hertz under an induction of 1 and 1.5 Tesla, as well as the induction obtained under the three values of magnetic fields taken as reference. .
  • the method according to the invention makes it possible, unexpectedly, to obtain from a magnetic sheet, on the one hand, high magnetic characteristics, and on the other hand mechanical characteristics comparable to those obtained by the method of the prior art.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Electromagnetism (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

This process, comprising successively after production under vacuum of a steel with a low silicon content: - a hot rolling operation followed by reeling; - a shot-blasting and pickling operation: - a cold rolling operation in one or more stages followed by annealing, to obtain a sheet of the final thickness, the final annealing being carried out under a decarbonising controlled atmosphere, is characterised in that the steel sheet has the following composition by weight: - carbon < 0.008% - silicon < 0.4% - manganese (0.05-0.4)% - sulphur < 0.01% - phosphorus < 0.19% - nitrogen < 0.01% - oxygen < 0.01%, the reeling following the hot rolling is carried out at a temperature above 600 DEG C and is itself followed by a heat treatment at a temperature above 700 DEG C.

Description

La présente invention concerne un procédé de fabrication d'une tôle d'acier magnétique à grains non orientés dit de "fully process" et la tôle obtenue par ce procédé.The present invention relates to a method of manufacturing a sheet of magnetic steel with non-oriented grain called "fully process" and the sheet obtained by this process.

On connaît un procédé comportant successivement, après élaboration sous vide d'un acier au silicium :

  • une opération de laminage à chaud suivie d'un bobinage;
  • une opération de grenaillage et de décapage acide;
  • une opération de laminage à froid en une ou plusieurs étapes suivie(s) d'un recuit pour obtenir une tôle à l'épaisseur finale, le recuit final étant réalisé sous atmosphère contrôlée décarburante.
A process is known which comprises successively, after vacuum production of a silicon steel:
  • a hot rolling operation followed by a winding;
  • an acid blasting and pickling operation;
  • a cold rolling operation in one or more stages followed by annealing to obtain a sheet of final thickness, the final annealing being carried out under a decarburizing controlled atmosphere.

Un tel procédé est connu et utilisé couramment dans le domaine de la réalisation de tôles magnétiques à grains non orientés.Such a method is known and commonly used in the field of making magnetic sheets with non-oriented grains.

Les tôles magnétiques dites à grains non orientés, c'est-à-dire ayant des propriétés magnétiques isotropes sont plus particulièrement destinées à la construction de dispositifs électromagnétiques dans lesquels le flux magnétique généré par les enroulements électriques n'est pas constant, comme par exemple dans les machines tournantes. Certains transformateurs utilisés dans le domaine de l'électroménager utilisent ce type de qualité pour des raisons économiques.Magnetic sheets known as non-oriented grain, that is to say having isotropic magnetic properties are more particularly intended for the construction of electromagnetic devices in which the magnetic flux generated by the electrical windings is not constant, such as for example in rotating machines. Some transformers used in the household appliance sector use this type of quality for economic reasons.

Ces dispositifs électromagnétiques sont constitués de tôles découpées et assemblées. Ces dernières ont un degré d'efficacité qui s'évalue en fonction de deux paramètres qui sont le niveau d'induction d'une part, et les pertes totales spécifiques, d'autre part.These electromagnetic devices consist of cut and assembled sheets. The latter have a degree of efficiency which is evaluated according to two parameters which are the level of induction on the one hand, and the specific total losses, on the other hand.

L'induction est limitée par l'aimantation à saturation des tôles et cette aimantation est d'autant plus élevée que le matériau est riche en fer. Cependant, il est nécessaire d'augmenter la résistivité de l'acier par addition de silicium et/ou d'aluminium afin de diminuer les pertes par courant de Foucault. L'élaboration sous vide permet d'améliorer la propreté et la pureté de l'acier et de réduire ainsi les pertes par hystérésis.The induction is limited by the saturation magnetization of the sheets and this magnetization is higher the higher the material is rich in iron. However, it is necessary to increase the resistivity of the steel by addition of silicon and / or aluminum in order to reduce the losses by eddy current. Vacuum processing improves the cleanliness and purity of the steel and thus reduces losses by hysteresis.

Aussi, il est nécessaire de trouver un compromis entre les tôles à forte aimantation à saturation et à faibles pertes.Also, it is necessary to find a compromise between sheets with strong saturation magnetization and low losses.

Les tôles à grains non orientés élaborées avec un acier dont la teneur en silicium est d'environ 3% ont actuellement les meilleures caractéristiques magnétiques de perte et une aimantation à saturation moins élevée que les tôles magnétiques dont l'acier ne contient pas ou peu de silicium.Non-oriented grain sheets made from steel with a silicon content of about 3% currently have the best magnetic loss characteristics and a lower saturation magnetization than magnetic sheets whose steel contains little or no silicon.

Dans certains domaines d'applications industrielles, où le choix technique d'un dispositif est un compromis entre ses performances techniques et son coût, on utilise des tôles magnétiques à grains non orientés élaborées avec un acier ne contenant, dans sa composition, qu'une très faible teneur en silicium, c'est-à-dire une teneur inférieure à 0,5%.In certain fields of industrial applications, where the technical choice of a device is a compromise between its technical performance and its cost, magnetic sheets with non-oriented grains are used, made with a steel containing, in its composition, only one very low silicon content, that is to say a content of less than 0.5%.

Du fait que l'élaboration des tôles en acier sans silicium reste plus aisée, donc plus économique, les industriels préfèrent utiliser un tel acier et cherchent à améliorer les caractéristiques magnétiques des tôles obtenues.Because the production of steel sheets without silicon remains easier, and therefore more economical, manufacturers prefer to use such steel and seek to improve the magnetic characteristics of the sheets obtained.

On connaît ainsi par le document EP-A-0434641 une composition contenant 0,2 à 2 % de silicium mais aussi 0,2 à 0,5 % d'aluminium.Document EP-A-0434641 thus discloses a composition containing 0.2 to 2% of silicon but also 0.2 to 0.5% of aluminum.

Est par ailleurs connue par le document JP-A-58-204126 une composition dans laquelle la quantité totale de silicium et d'aluminium est inférieure ou égale à 1,5 %.Is also known from document JP-A-58-204126 a composition in which the total amount of silicon and aluminum is less than or equal to 1.5%.

Dans un autre domaine de fabrication de tôles magnétiques, dites à grains orientés, le procédé de fabrication comprend, après élaboration d'un acier contenant dans sa composition une teneur en silicium d'environ 3%, du soufre, du manganèse, de l'aluminium et de l'azote pour former des inhibiteurs tels que le sulfure de manganèse ou le nitrure d'aluminium :

  • un laminage à chaud;
  • une opération dite de recuit initial consistant à élever la température de la tôle laminée à chaud pendant quelques minutes sous atmosphère contrôlée;
  • une opération de grenaillage et de décapage acide;
  • une opération de laminage à froid suivie de recuits en atmosphère contrôlée.
In another field of manufacturing magnetic sheets, known as oriented grain, the manufacturing process comprises, after production of a steel containing in its composition a silicon content around 3%, sulfur, manganese, aluminum and nitrogen to form inhibitors such as manganese sulfide or aluminum nitride:
  • hot rolling;
  • a so-called initial annealing operation consisting in raising the temperature of the hot-rolled sheet for a few minutes under a controlled atmosphere;
  • an acid blasting and pickling operation;
  • a cold rolling operation followed by annealing in a controlled atmosphere.

Obtenues par ce procédé, les tôles dites à grains orientés ont une très forte proportion de grains ayant une orientation (110). [001]. Ces tôles possèdent d'excellentes propriétés magnétiques dans la direction du laminage. Elles sont anisotropes, c'est-à-dire que leurs propriétés dépendent de la direction de laminage. C'est ainsi que, par exemple, les pertes d'une tôle magnétique de composition courante, de 0,35 mm d'épaisseur, sont trois fois plus élevées dans la direction perpendiculaire au sens du laminage que dans la direction du laminage.Obtained by this process, the so-called oriented grain sheets have a very high proportion of grains having an orientation (110). [001]. These sheets have excellent magnetic properties in the direction of rolling. They are anisotropic, that is to say that their properties depend on the direction of rolling. Thus, for example, the losses of a magnetic sheet of common composition, 0.35 mm thick, are three times higher in the direction perpendicular to the direction of rolling than in the direction of rolling.

Les tôles à propriétés magnétiques anisotropes présentent donc l'inconvénient de ne pouvoir être employées que pour les applications dans lesquelles les lignes de champ magnétique correspondent à la direction du laminage. Il s'agit donc de les utiliser pour des machines statiques telles que les transformateurs.Sheets with anisotropic magnetic properties therefore have the disadvantage that they can only be used for applications in which the magnetic field lines correspond to the direction of rolling. It is therefore a question of using them for static machines such as transformers.

Dans l'élaboration des tôles à grains orientés, l'opération initiale de recuit après le laminage à chaud a pour fonction d'influer sur l'état des précipités, par exemple de MnS et/ou de AlN par rapport à la microstructure des tôles de façon à favoriser le développement ultérieur de la croissance de grains orientés pour former une texture de GOSS.In the preparation of oriented grain sheets, the initial annealing operation after hot rolling has the function of influencing the state of the precipitates, for example MnS and / or AlN with respect to the microstructure of the sheets so as to promote the further development of the growth of oriented grains to form a GOSS texture.

L'invention a pour but d'améliorer les caractéristiques magnétiques de tôles à grains non orientés réalisées avec un acier ne contenant que très peu de silicium, c'est-à-dire de réduire les pertes magnétiques et d'augmenter l'aimantation sous un champ magnétique déterminé.The object of the invention is to improve the magnetic characteristics of non-oriented grain sheets made from steel containing very little silicon, that is to say to reduce the magnetic losses and to increase the magnetization under a determined magnetic field.

Elle a pour objet un procédé d'élaboration de tôles magnétiques à grains non orientés tel que défini précédemment et dans lequel la tôle d'acier a la composition pondérale suivante :

  • Carbone ≤ 0,008 %
  • Silicium ≤ 0,4 %
  • Manganèse (0,05-0,4) %
  • Al < 0,05 %
  • Soufre < 0,01 %
  • Phosphore < 0,19 %
  • Azote < 0,01 %
  • Oxygène < 0,01%, le reste étant du fer,
le bobinage suivant le laminage à chaud est effectué à une température supérieure à 600°C et lui-même suivi d'un traitement thermique à une température supérieure à 700°C, sous atmosphère contrôlée constituée exclusivement d'azote.Its subject is a process for producing magnetic sheets with non-oriented grains as defined above and in which the steel sheet has the following composition by weight:
  • Carbon ≤ 0.008%
  • Silicon ≤ 0.4%
  • Manganese (0.05-0.4)%
  • Al <0.05%
  • Sulfur <0.01%
  • Phosphorus <0.19%
  • Nitrogen <0.01%
  • Oxygen <0.01%, the rest being iron,
the winding following the hot rolling is carried out at a temperature above 600 ° C and itself followed by a heat treatment at a temperature above 700 ° C, under a controlled atmosphere consisting exclusively of nitrogen.

Ce procédé contribue à une amélioration des qualités magnétiques, c'est-à-dire une diminution des pertes totales spécifiques et aussi une augmentation de l'aimantation.This process contributes to an improvement in the magnetic qualities, that is to say a reduction in the specific total losses and also an increase in the magnetization.

Selon d'autres caractéristiques :

  • l'opération de grenaillage et de décapage acide est réalisée après bobinage et traitement thermique.
  • la température de bobinage est comprise dans l'intervalle (600-750)°C et de préférence entre (600 et 680)°C,
  • le traitement thermique préalable au laminage à froid comprend :
  • une mise sous atmosphère contrôlée,
  • une élévation en température comprise dans l'intervalle 700-1100°C,
  • un maintien en température pendant un temps compris dans l'intervalle de 1 à 10 minutes.
According to other characteristics:
  • the shot peening and acid pickling operation is carried out after winding and heat treatment.
  • the winding temperature is in the range (600-750) ° C and preferably between (600 and 680) ° C,
  • the heat treatment prior to cold rolling includes:
  • placing under a controlled atmosphere,
  • a temperature rise in the range 700-1100 ° C,
  • maintaining the temperature for a time in the range of 1 to 10 minutes.

Par ailleurs et de préférence :

  • la température du traitement thermique préalable est comprise dans l'intervalle 800-1050°C :
  • le temps de maintien de la température du traitement thermique est compris dans l'intervalle de 1 à 4 minutes.
Furthermore and preferably:
  • the temperature of the preliminary heat treatment is in the range 800-1050 ° C:
  • the heat treatment temperature holding time is in the range of 1 to 4 minutes.

L'invention concerne également la tôle magnétique à grains non orientés obtenue selon le procédé et ayant les caractéristiques suivantes :

  • elle a la composition pondérale suivante :
    • Carbone ≤ 0,008 %
    • Silicium ≤ 0,4 %
    • Manganèse (0,05-0,4) %
    • Al < 0,05 %
    • Soufre < 0,01 %
    • Phosphore < 0,19 %
    • Azote < 0,01 %
    • Oxygène < 0,01 %, le reste de la composition étant du fer et des impuretés inévitables
    • pour une tôle ayant une épaisseur d'environ 0,5mm, les pertes spécifiques à 1,5 Tesla et 50 Hertz sont inférieures à 6,3 W/Kg et l'aimantation est supérieure à 1,65; 1,74; 1,85 Tesla, respectivement sous des champs magnétiques de 2500, 5000, 10000 A/m.
    • de préférence les pertes spécifiques à 1,5 Tesla et 50 Hertz sont inférieures à 5,1 W/kg et l'aimantation est supérieure à 1,68, 1,77; 1,89 Tesla, respectivement sous des champs magnétiques de 2500, 5000, 10000 A/m.
    • pour une tôle ayant une épaisseur d'environ 0,65 mm, les pertes spécifiques à 1,5 Tesla et 50 Hertz sont inférieures à 7,5 W/kg et l'aimantation est supérieure à 1,66, 1,75, 1,86 Tesla respectivement sous des champs de 2500, 5000, 10000 A/m.
    • de préférence, les pertes spécifiques à 1,5 Tesla et 50 Hertz sont inférieures à 7,1 W/Kg et l'aimantation est supérieure à 1,67; 1,76; 1,88 Tesla, respectivement sous des champs magnétiques de 2500, 5000, 10000 A/m.
The invention also relates to the magnetic sheet with non-oriented grains obtained according to the process and having the following characteristics:
  • it has the following weight composition:
    • Carbon ≤ 0.008%
    • Silicon ≤ 0.4%
    • Manganese (0.05-0.4)%
    • Al <0.05%
    • Sulfur <0.01%
    • Phosphorus <0.19%
    • Nitrogen <0.01%
    • Oxygen <0.01%, the rest of the composition being iron and unavoidable impurities
    • for a sheet having a thickness of approximately 0.5 mm, the specific losses at 1.5 Tesla and 50 Hertz are less than 6.3 W / Kg and the magnetization is greater than 1.65; 1.74; 1.85 Tesla, respectively under magnetic fields of 2500, 5000, 10000 A / m.
    • preferably the specific losses at 1.5 Tesla and 50 Hertz are less than 5.1 W / kg and the magnetization is greater than 1.68, 1.77; 1.89 Tesla, respectively under magnetic fields of 2500, 5000, 10000 A / m.
    • for a sheet having a thickness of approximately 0.65 mm, the specific losses at 1.5 Tesla and 50 Hertz are less than 7.5 W / kg and the magnetization is greater than 1.66, 1.75, 1 , 86 Tesla respectively under fields of 2500, 5000, 10000 A / m.
    • preferably, the specific losses at 1.5 Tesla and 50 Hertz are less than 7.1 W / Kg and the magnetization is greater than 1.67; 1.76; 1.88 Tesla, respectively under magnetic fields of 2500, 5000, 10000 A / m.

Les caractéristiques magnétiques et mécaniques obtenues dans les essais comparatifs qui suivent sont données à titre d'exemple non limitatif, et mettent bien en évidence l'invention.The magnetic and mechanical characteristics obtained in the comparative tests which follow are given by way of nonlimiting example, and clearly demonstrate the invention.

Dans un premier exemple de réalisation de l'invention, l'acier utilisé pour la fabrication de tôles magnétiques en "fully process" a la composition pondérale suivante :

  • Carbone ≤ 0,008%
  • Silicium ≤ 0,4%
  • Soufre < 0,01%
  • Aluminium < 0,05%
  • Phosphore < 0,19%
  • Manganèse < (0,05-0,4)%
  • Azote < 0,010%
  • Oxygène < 0,01 %, le reste étant du fer et des impuretés inévitables.
In a first embodiment of the invention, the steel used for the manufacture of magnetic sheets in "fully process" has the following weight composition:
  • Carbon ≤ 0.008%
  • Silicon ≤ 0.4%
  • Sulfur <0.01%
  • Aluminum <0.05%
  • Phosphorus <0.19%
  • Manganese <(0.05-0.4)%
  • Nitrogen <0.010%
  • Oxygen <0.01%, the rest being iron and unavoidable impurities.

La présence de manganèse dans la composition de l'acier est nécessaire pour obtenir une bonne ductilité à chaud et à froid en présence de silicium.The presence of manganese in the composition of the steel is necessary to obtain good hot and cold ductility in the presence of silicon.

L'acier est élaboré sous vide et coulé en continu sous forme de brames. La tôle est réalisée lors de l'opération de laminage à chaud après un laminage à des brames au train à bande.The steel is produced under vacuum and continuously cast in the form of slabs. The sheet is produced during the hot rolling operation after rolling with slabs using a band train.

Selon l'invention la bande d'acier laminée à chaud est soumise avant l'opération de laminage à froid à un bobinage à une température de 650°C et à un traitement thermique préalable au laminage à froid, consistant, dans un essai donnant de bonnes caractéristiques, à :

  • une mise à température de 800°C pendant 2 minutes sous atmosphère d'azote;
  • un laminage à froid en une ou plusieurs étapes pour la mise à épaisseur de la tôle, la tôle ainsi laminée étant soumise à un recuit final en continu à 880°C sous atmosphère décarburante telle que NH3 craqué.
According to the invention, the hot rolled steel strip is subjected before the cold rolling operation to a winding at a temperature of 650 ° C. and to a heat treatment prior to cold rolling, consisting, in a test giving good characteristics, to:
  • a temperature rise of 800 ° C for 2 minutes under a nitrogen atmosphere;
  • cold rolling in one or more stages for thickening the sheet, the sheet thus laminated being subjected to a final annealing continuously at 880 ° C. under a decarburizing atmosphere such as cracked NH 3 .

Le tableau I regroupe les valeurs des caractéristiques magnétiques obtenues dans une série d'essais de variation des conditions du traitement thermique préalable au laminage à froid.Table I groups together the values of the magnetic characteristics obtained in a series of tests for variation of the conditions of the heat treatment prior to cold rolling.

Les essais ont été réalisés en faisant varier la température du traitement de 700°C à 1100°C, les temps de maintien en température étant variables de 1 à 5 minutes.The tests were carried out by varying the temperature of the treatment from 700 ° C. to 1100 ° C., the temperature holding times being variable from 1 to 5 minutes.

Les autres paramètres utilisés dans le procédé sont :

  • une atmosphère d'azote lors du traitement thermique préalable;
  • un laminage à froid pour l'obtention d'une épaisseur finale de la tôle d'environ 0,5 mm;
  • un recuit final à 880°C sous NH3 craqué pendant 2 minutes avec un point de rosée à + 20°C.
The other parameters used in the process are:
  • a nitrogen atmosphere during the preliminary heat treatment;
  • cold rolling to obtain a final sheet thickness of about 0.5 mm;
  • final annealing at 880 ° C under NH 3 cracked for 2 minutes with a dew point at + 20 ° C.

Les caractéristiques magnétiques d'induction ont été mesurées sous trois champs magnétiques de 2500, 5000 et 10000 A/m, alors que les caractéristiques de pertes totales spécifiques sont données à 1 et 1,5 Tesla. TABLEAU I TRAITEMENT PREALABLE EPAISSEUR APRES LAMINAGE A FROID RECUIT FINAL B (TESLA) pour H (A/m) W/kg (50 Hz) T° de PALIER (°C) Temps de maintien (mn) 2.500 5.000 10.000 1T 1,5T 700 1 880°C 1,626 1,715 1,835 700 2 0,5 mm 2 mn NH3 1,631 1,718 1,838 2,36 5,26 700 5 craqué 1,638 1,717 1,837 800 1 880°C 1,696 1,787 1,903 2,15 4,59 800 2 0,5 mm 2 mn NH3 1,699 1,788 1,904 2,12 4,57 800 5 craqué 1,708 1,793 1,909 2,11 4,54 1050 1 880°C 1,695 1,782 1,899 1050 2 0,5 mn 2 mn NH3 1,697 1,781 1,897 1050 5 craqué 1,697 1,784 1,899 2,12 4,57 1100 1 880°C 1,700 1,787 1,898 1100 2 0,5 mn 2 mn NH3 1,697 1,785 1,899 1100 5 craqué 1,698 1,786 1,899 2,31 4,96 880°C SANS TRAITEMENT 0,5 mm 2 mn NH3 1,624 1,713 1,832 2,31 5,21 craqué The magnetic induction characteristics were measured under three magnetic fields of 2500, 5000 and 10000 A / m, while the specific total loss characteristics are given at 1 and 1.5 Tesla. TABLE I PRE-TREATMENT THICKNESS AFTER COLD ROLLING Final annealing B (TESLA) for H (A / m) W / kg (50 Hz) BEARING T ° (° C) Holding time (min) 2,500 5,000 10,000 1T 1.5T 700 1 880 ° C 1.626 1,715 1,835 700 2 0.5mm 2 min NH3 1.631 1,718 1.838 2.36 5.26 700 5 cracked 1.638 1,717 1.837 800 1 880 ° C 1,696 1.787 1.903 2.15 4.59 800 2 0.5mm 2 min NH3 1,699 1,788 1.904 2.12 4.57 800 5 cracked 1.708 1.793 1.909 2.11 4.54 1050 1 880 ° C 1.695 1.782 1,899 1050 2 0.5 min 2 min NH3 1,697 1.781 1.897 1050 5 cracked 1,697 1,784 1,899 2.12 4.57 1100 1 880 ° C 1,700 1.787 1.898 1100 2 0.5 min 2 min NH3 1,697 1,785 1,899 1100 5 cracked 1,698 1,786 1,899 2.31 4.96 880 ° C WITHOUT TREATMENT 0.5mm 2 min NH3 1,624 1,713 1,832 2.31 5.21 cracked

Les résultats des essais montrent par comparaison avec les caractéristiques d'un échantillon n'ayant pas subi de traitement que le traitement préalable permet d'augmenter, d'une part les inductions d'environ 5% et d'autre part de réduire les pertes d'environ 12%.The results of the tests show, by comparison with the characteristics of a sample which has not undergone treatment, that the preliminary treatment makes it possible to increase, on the one hand the inductions of about 5% and on the other hand to reduce the losses about 12%.

Ces essais mettent en évidence que les meilleures caractéristiques magnétiques des tôles sont obtenues par un traitement préalable compris entre 800 et 1050°C pour les tôles d'acier ayant la composition citée ci-dessus.These tests show that the best magnetic characteristics of the sheets are obtained by a preliminary treatment of between 800 and 1050 ° C. for the steel sheets having the composition cited above.

Dans un deuxième exemple de réalisation, avec un acier ayant la composition suivante :

C =
0,004
Si =
0,280
S =
0,009
Al =
0,020
P =
0,140
Mn =
0,300
N2 =
0,007
O2 =
0,005
traité dans les mêmes conditions que l'acier de l'exemple 1 ci-dessus, il a été réalisé des essais mesurant des caractéristiques d'inductions sous trois champs magnétiques de 2500, 5000 et 10000 A/m et les pertes totales spécifiques.In a second example of embodiment, with a steel having the following composition:
C =
0.004
If =
0.280
S =
0.009
Al =
0.020
P =
0.140
Mn =
0.300
N 2 =
0.007
O 2 =
0.005
treated under the same conditions as the steel of example 1 above, tests were carried out measuring inductive characteristics under three magnetic fields of 2500, 5000 and 10000 A / m and the specific total losses.

Le tableau II regroupe, pour deux épaisseurs de tôles magnétiques, les caractéristiques de pertes en W/Kg à 50 Hertz sous une induction de 1 et 1,5 Tesla, ainsi que l'induction obtenue sous les trois valeurs de champs magnétiques pris en référence.

Figure imgb0001
Table II groups together, for two thicknesses of magnetic sheets, the loss characteristics in W / Kg at 50 Hertz under an induction of 1 and 1.5 Tesla, as well as the induction obtained under the three values of magnetic fields taken as reference. .
Figure imgb0001

Le procédé selon l'invention permet, de manière inattendue, d'obtenir d'une tôle magnétique d'une part de hautes caractéristiques magnétiques, et d'autre part des caractéristiques mécaniques comparables à celles obtenues par le procédé de l'art antérieur.The method according to the invention makes it possible, unexpectedly, to obtain from a magnetic sheet, on the one hand, high magnetic characteristics, and on the other hand mechanical characteristics comparable to those obtained by the method of the prior art.

Claims (10)

  1. Process for manufacturing unoriented-grain magnetic steel sheet, called the "fully process", which includes, in succession, after vacuum smelting a silicon steel:
    - a hot-rolling operation followed by coiling;
    - a shot-peening and pickling operation;
    - a cold-rolling operation, including at least one step followed by an anneal, in order to obtain a sheet with the final thickness, the final anneal being carried out in a decarburizing controlled atmosphere; in which process:
    - the steel sheet has the following composition by weight:
    - carbon ≤ 0.008 %
    - silicon ≤ 0.4 %
    - manganese (0.05-0.4) %
    - Al < 0.05 %
    - sulphur < 0.01%
    - phosphorus < 0.19 %
    - nitrogen < 0.01%
    - oxygen < 0.01%,
    the balance of the composition being iron and inevitable impurities;
    - the coiling which follows the hot rolling is performed at a temperature above 600°C and is itself followed by a heat treatment at a temperature above 700°C, under a controlled atmosphere, consisting essentially of nitrogen.
  2. Process according to Claim 1, characterized in that the shot-peening and acid pickling operation is carried out after coiling and heat treatment.
  3. Process according to Claim 1, characterized in that the coiling temperature lies within the range (600-750)°C and preferably between 600 and 680°C.
  4. Process according to any one of Claims 1 to 3, characterized in that the heat treatment prior to the cold rolling comprises:
    - exposure to a controlled atmosphere;
    - a temperature rise lying within the range 700-1100°C;
    - a temperature hold for a time lying within the range of from 1 to 10 minutes.
  5. Process according to either of Claims 1 and 4, characterized in that the temperature of the heat treatment prior to the cold rolling lies between 800 and 1050°C.
  6. Process according to any one of Claims 1 to 5, characterized in that the temperature-hold time of the prior heat treatment is from 1 to 5 minutes.
  7. Unoriented-grain magnetic sheet obtained by the process according to any one of Claims 1 to 6, characterized in that it has the following composition by weight:
    - carbon ≤ 0.008 %
    - silicon ≤ 0.4 %
    - manganese (0.05-0.4) %
    - Al < 0.05 %
    - sulphur < 0.01 %
    - phosphorus < 0.19 %
    - nitrogen < 0.01 %
    - oxygen < 0.01%,
    the balance of the composition being iron and inevitable impurities; and in that, for a sheet having a thickness of approximately 0.5 mm, the specific losses at 1.5 tesla and 50 hertz are less than 6.3 W/Kg and the magnetization is greater than 1.65, 1.74 and 1.85 tesla, respectively, under magnetic fields of 2500, 5000 and 10,000 A/m.
  8. Sheet according to Claim 7, characterized in that the specific losses at 1.5 tesla and 50 hertz are less than 5.1 W/Kg and the magnetization is greater than 1.68, 1.77 and 1.89 tesla, respectively, under magnetic fields of 2500, 5000 and 10,000 A/m.
  9. Unoriented-grain magnetic sheet obtained by the process according to any one of Claims 1 to 6, characterized in that it has the following composition by weight:
    - carbon ≤ 0.008 %
    - silicon ≤ 0.4 %
    - manganese (0.05-0.4) %
    - Al < 0.05 %
    - sulphur < 0.01%
    - phosphorus < 0.19 %
    - nitrogen < 0.01 %
    - oxygen < 0.01%,
    the balance of the composition being iron and inevitable impurities; and in that, for a sheet having a thickness of approximately 0.65 mm, the specific losses at 1.5 tesla and 50 hertz are less than 7.5 W/Kg and the magnetization is greater than 1.66, 1.75 and 1.86 tesla, respectively, under fields of 2500, 5000 and 10,000 A/m.
  10. Sheet according to Claim 9, characterized in that the specific losses at 1.5 tesla and 50 hertz are less than 7.1 W/Kg and the magnetization is greater than 1.67, 1.76 and 1.88 tesla, respectively, under magnetic fields of 2500, 5000 and 10,000 A/m.
EP91402117A 1990-07-30 1991-07-29 Process for manufacturing grain non oriented magnetic steel sheet and sheet obtained thereby Expired - Lifetime EP0469980B1 (en)

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FR9009694A FR2665181B1 (en) 1990-07-30 1990-07-30 PROCESS FOR PRODUCING MAGNETIC STEEL SHEET WITH NON-ORIENTED GRAINS AND SHEET OBTAINED BY THIS PROCESS.
FR9009694 1990-07-30

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19807122A1 (en) * 1998-02-20 1999-09-09 Thyssenkrupp Stahl Ag Process for the production of non-grain oriented electrical sheet
DE102021115174A1 (en) 2021-06-11 2021-11-11 Technische Universität Bergakademie Freiberg, Körperschaft des öffentlichen Rechts Process for the production of a higher permeability, non-grain oriented electrical steel sheet and its use

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19930519C1 (en) * 1999-07-05 2000-09-14 Thyssenkrupp Stahl Ag Non-textured electrical steel sheet, useful for cores in rotary electrical machines such as motors and generators, is produced by multi-pass hot rolling mainly in the two-phase austenite-ferrite region
BE1006599A6 (en) * 1993-01-29 1994-10-25 Centre Rech Metallurgique Method of manufacturing a plate hot rolled steel having high magnetic properties.
DE4302813C2 (en) * 1993-02-02 1996-01-18 Dresden Ev Inst Festkoerper Process for the production of a cube surface texture ((100) [Okl]) in electrical sheets
BE1007927A3 (en) * 1994-02-07 1995-11-21 Cockerill Rech & Dev Method for producing mild steel.
FR2744135B1 (en) * 1996-01-25 1998-02-27 Usinor Sacilor PROCESS FOR PRODUCING MAGNETIC STEEL SHEET WITH NON-ORIENTED GRAINS AND SHEET OBTAINED BY THE PROCESS
DE19918484C2 (en) * 1999-04-23 2002-04-04 Ebg Elektromagnet Werkstoffe Process for the production of non-grain oriented electrical sheet
DE10221793C1 (en) 2002-05-15 2003-12-04 Thyssenkrupp Electrical Steel Ebg Gmbh Non-grain oriented electrical steel or sheet and process for its manufacture

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2057500A (en) * 1979-09-07 1981-04-01 British Steel Corp Improvements in electro magnetic steels
EP0263413A2 (en) * 1986-09-29 1988-04-13 Nippon Kokan Kabushiki Kaisha Non-oriented electrical steel sheets and producing non-oriented steel sheets
EP0434641A2 (en) * 1989-12-22 1991-06-26 CENTRO SVILUPPO MATERIALI S.p.A. Process for the production of semiprocessed non oriented grain electrical steel

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1531090A (en) * 1966-07-13 1968-06-28 Koninklijke Hoogovens En Staal Dynamo steel fabrication process
JPS4819766B1 (en) * 1970-03-30 1973-06-15
JPS58117828A (en) * 1981-12-28 1983-07-13 Nippon Steel Corp Production of semi-process nondirectional electrical sheet having low iron loss and high magnetic flux density
JPS58204126A (en) * 1982-05-21 1983-11-28 Kawasaki Steel Corp Production of nondirectional electrical steel strip having excellent magnetic characteristic
JPH0788530B2 (en) * 1987-06-24 1995-09-27 住友金属工業株式会社 Manufacturing method of non-oriented electrical steel sheet with high magnetic flux density
JP2501219B2 (en) * 1987-12-25 1996-05-29 川崎製鉄株式会社 Non-oriented electrical steel sheet manufacturing method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2057500A (en) * 1979-09-07 1981-04-01 British Steel Corp Improvements in electro magnetic steels
EP0263413A2 (en) * 1986-09-29 1988-04-13 Nippon Kokan Kabushiki Kaisha Non-oriented electrical steel sheets and producing non-oriented steel sheets
EP0434641A2 (en) * 1989-12-22 1991-06-26 CENTRO SVILUPPO MATERIALI S.p.A. Process for the production of semiprocessed non oriented grain electrical steel

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Patent Abstracts of Japan, vol. 12 no. 155 (C-494),12.05.88, & JP-A-62 267 421 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19807122A1 (en) * 1998-02-20 1999-09-09 Thyssenkrupp Stahl Ag Process for the production of non-grain oriented electrical sheet
DE19807122C2 (en) * 1998-02-20 2000-03-23 Thyssenkrupp Stahl Ag Process for the production of non-grain oriented electrical sheet
DE102021115174A1 (en) 2021-06-11 2021-11-11 Technische Universität Bergakademie Freiberg, Körperschaft des öffentlichen Rechts Process for the production of a higher permeability, non-grain oriented electrical steel sheet and its use

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ATE140271T1 (en) 1996-07-15
DE69120738T2 (en) 1996-11-21
FR2665181B1 (en) 1994-05-27
ES2091889T3 (en) 1996-11-16
DE69120738D1 (en) 1996-08-14
GR3020930T3 (en) 1996-12-31
EP0469980A1 (en) 1992-02-05

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