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EP2979281B1 - Electrical steel sheet with a coating improving the electrical insulation and method of its manufacture - Google Patents

Electrical steel sheet with a coating improving the electrical insulation and method of its manufacture Download PDF

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Publication number
EP2979281B1
EP2979281B1 EP14721254.2A EP14721254A EP2979281B1 EP 2979281 B1 EP2979281 B1 EP 2979281B1 EP 14721254 A EP14721254 A EP 14721254A EP 2979281 B1 EP2979281 B1 EP 2979281B1
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EP
European Patent Office
Prior art keywords
layer
steel sheet
tantalum
titanium
oxide
Prior art date
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EP14721254.2A
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German (de)
French (fr)
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EP2979281A1 (en
Inventor
Jens Dahl Jensen
Axel MÖHLE
Ralph Reiche
Manuela Schneider
Oliver Stier
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Siemens AG
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Siemens AG
Siemens Corp
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    • 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
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • 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
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • H01F1/18—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets with insulating coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/60—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising

Definitions

  • the invention relates to an electrical sheet with an electrical insulation improving layer.
  • Such electrical sheets are used according to the prior art, for example in electric drives in the construction of stators.
  • the materials used are regulated by the standard EN 10106 (1995).
  • the materials mentioned in this standard provide a wide range of products to meet the needs of different applications.
  • the usable materials range from low-alloyed steel with excellent magnetic permeability, good thermal conductivity and punchability to higher-alloyed steels with very low core losses even at higher frequencies.
  • the base of the alloy is iron.
  • Coatings for electrical sheets can be taken from the standard EN 10342 (from 2005).
  • aluminum layers on ferroalloy components may be used to reduce the nitrogen content in the component.
  • an intermediate layer of aluminum nitride is formed between the aluminum layer and the component, which also acts as a diffusion barrier layer, so that aluminum can not diffuse into the component.
  • aluminum it is also possible to use other metals which are capable of forming nitrides with nitrogen. Examples of such metals include titanium and tantalum.
  • the object of the invention is therefore to provide an electrical sheet which is also suitable for use under severe corrosive conditions.
  • the layer of a metal oxide containing mainly titanium oxide or tantalum oxide, and that the electrical steel has a diffusion zone in which the metal of the metal oxide is diffused into the material of the electric sheet and the the layer adjoins. Due to the fact that the oxide layer adjoins a diffusion layer, the adhesion of the oxide layer is advantageously greatly improved.
  • the use of metals, titanium or tantalum causes the spontaneously forming on the surface of the electrical sheet oxide layer is very resistant to corrosive media. This also makes use under extreme corrosive conditions such. B. sour gas possible. For example, motor pumps can be operated, which are used for the promotion of natural gas in the subsea area.
  • the oxide layer can also be produced by an electrochemical treatment of the surface (more on this in the following).
  • the diffusion zone following the oxide layer has two advantages. On the one hand, the diffusion zone improves the adhesion of the oxide layer, since the transition between the oxide layer and the matrix material of the electrical steel, a steel alloy, takes place continuously, which reduces the formation of stresses. In addition, it is advantageously possible that in case of damage to the oxide layer, the material contained in the diffusion layer of titanium or tantalum can be used to passivate the damaged area. For this purpose, the metal in question diffuses to the surface, where a renewed passivation takes place. The corrosion protection is thereby advantageously retained.
  • the layer has a thickness of at least 5 and at most 10 microns. These are layer thicknesses of the oxide layer, which allow effective corrosion protection and in their production due to the small thickness advantageously require low production costs and low material usage.
  • the diffusion zone within a distance of 2 microns from the interface to the layer has a content of titanium or tantalum of more than 50% by weight.
  • These are alloy contents which advantageously permit diffusion-induced transport of titanium or tantalum to damaged areas (as already described).
  • contents of up to 100% of titanium or tantalum can also occur directly below the oxide layer.
  • the invention relates to a method for treating an electric sheet, in which the electrical sheet is coated with an electrical insulation improving layer.
  • the prior art has already been discussed. The task which results from this is to specify a method with which the treatment of electrical steel sheets is possible and which produces products which ensure sufficient corrosion protection even under strongly corrosive influences.
  • a diffusion zone is produced on the surface of the electric sheet, wherein as a metal tantalum or titanium diffused into the surface, wherein the first step as a PVD process in an inert gas atmosphere a subsequent heat treatment is performed.
  • the metal, tantalum or titanium on the surface is converted into the associated metal oxide, titanium oxide or tantalum oxide, wherein a layer of the metal oxide is formed and remains in the diffusion zone, a residual content of the metal of the metal oxide.
  • the residual content remains on the metal of the metal oxide, whereby, as already explained, the adhesion of the oxide layer is improved.
  • a depot is formed by the diffusion zone on the corresponding material, which is available in case of injuries of the oxide layer to heal the injury by spontaneous passivation.
  • PVD processes are advantageously easy to handle.
  • Both titanium and tantalum can be deposited on steel by using suitable target materials.
  • titanium is deposited in multiple ways by PVD processes to make tool coatings, usually in a reactive nitrogen atmosphere, to produce titanium nitride. If instead an inert gas atmosphere is selected, pure titanium is deposited. Tantalum can also be easily deposited on steel.
  • Such a method is for example in the EP 77 535 A1 described.
  • the deposition of titanium for example, by spraying or powder coating done, such as the Derwent Abstract with the Accession Number 1978-43006 A (corresponding to JP 53-50019 A ) can be seen.
  • the powder processes are also referred to as packing processes, in which case the diffusion layers are formed by diffusing the tantalum into the workpiece.
  • the diffusion layer thus arises immediately, whereas in PVD processes after the coating process, a heat treatment has to take place, which leads to an inward diffusion of the tantalum or titanium into the matrix of the electrical sheet.
  • Parameters for such diffusion treatments are well known and can be found, for example, in the Derwent Abstract with the Accession Number 1984-104398 (corresponding to US Pat JP 59-47371 A ) remove.
  • electrochemical coatings for example in a salt bath, are also conceivable in principle, or else coating by means of CVD.
  • the diffusion zone before the formation of the layer within a distance of 5 microns from the interface to the layer has a content of titanium or tantalum of more than 50% by weight. It goes without saying that the diffusion zone must have a larger area with a high titanium or tantalum concentration before the formation of the layer, since a portion of the previously formed diffusion layer is converted into the oxide layer by oxidation of the titanium or tantalum. In order to still have enough material for a repair of the oxide layer in the matrix of the electrical steel available after this oxidation process, therefore, the proportion of titanium or tantalum must be sufficiently high.
  • FIGURE shows an embodiment of the electric sheet metal according to the invention in cross section.
  • an electric sheet 11 the top 12 and bottom 13 is provided in each case with a layer 14 of tantalum oxide.
  • This layer 14 is followed by a diffusion zone 15, which has a common interface 16 with the layer 12 of tantalum oxide. Behind the interface, the concentration of tantalum in the diffusion zone is well over 50%. This falls to the interior of the electric sheet 11 continues until the concentration is 0% by weight. In itself, therefore, a boundary between the actual electrical sheet 11 and the diffusion zone 15 can not really represent.
  • the figure shows the region in which the concentration of tantalum in the microstructure of the electrical sheet 11 is more than 50%.

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  • Power Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Soft Magnetic Materials (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Physical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)
  • Insulating Bodies (AREA)

Description

Die Erfindung betrifft ein Elektroblech mit einer die elektrische Isolation verbessernden Schicht.The invention relates to an electrical sheet with an electrical insulation improving layer.

Solche Elektrobleche werden gemäß dem Stand der Technik zum Beispiel bei elektrischen Antrieben beim Aufbau von Statoren verwendet. Die verwendeten Werkstoffe sind durch die Norm EN 10106 (von 1995) reglementiert. Die in dieser Norm genannten Werkstoffe ergeben ein weit gefächertes Produktsortiment, damit die Ansprüche unterschiedlicher Anwendungen befriedigt werden können. Die einsetzbaren Werkstoffe reichen von niedrig legiertem Stahl mit ausgezeichneter magnetischer Permeabilität, guter Wärmeleitfähigkeit und Stanzbarkeit bis hin zu höher legierten Stählen mit sehr geringen Ummagnetisierungsverlusten auch bei höheren Frequenzen. Die Legierungen der Norm enthalten als Legierungsbestandteile Kupfer (<= 0,02 %) Mangan (<= 1,2 %), Silizium (0,1 - 4,4 %), Aluminium (0,1 - 4,4 %), wobei die aus dem Siliziumgehalt und dem Doppelten des Aluminiumgehaltes gebildete Summe < 5 % ist, Phosphor (<= 0,15 %), Zinn (<= 0,2 %) und Antimon (<= 0,2 %). Die Basis der Legierung bildet Eisen.Such electrical sheets are used according to the prior art, for example in electric drives in the construction of stators. The materials used are regulated by the standard EN 10106 (1995). The materials mentioned in this standard provide a wide range of products to meet the needs of different applications. The usable materials range from low-alloyed steel with excellent magnetic permeability, good thermal conductivity and punchability to higher-alloyed steels with very low core losses even at higher frequencies. The alloys of the standard contain as their constituents copper (<= 0.02%) manganese (<= 1.2%), silicon (0.1 - 4.4%), aluminum (0.1 - 4.4%), wherein the sum formed from the silicon content and the double of the aluminum content is <5%, phosphorus (<= 0.15%), tin (<= 0.2%) and antimony (<= 0.2%). The base of the alloy is iron.

Zur Verbesserung der Eigenschaften der Elektrobleche wurden Beschichtungen entwickelt, welche die Isolation zwischen den einzelnen Blechlagen und die Bearbeitbarkeit verbessern. Die spezifischen Eigenschaften des verwendeten Materials müssen Einflussgrößen wie Korrosionsschutz, elektrische Isolation, Einfluss auf die Stanzbarkeit, Hitzebeständigkeit oder Schweißbarkeit berücksichtigen. Beschichtungen für Elektrobleche lassen sich der Norm EN 10342 (von 2005) entnehmen.In order to improve the properties of the electrical steel sheets, coatings have been developed which improve the insulation between the individual sheet metal layers and the machinability. The specific properties of the material used must take account of factors such as corrosion protection, electrical insulation, influence on punchability, heat resistance or weldability. Coatings for electrical sheets can be taken from the standard EN 10342 (from 2005).

Die in den oben genannten Normen verfügbaren Elektrobleche und deren Beschichtungen sind, wie sich gezeigt hat, jedoch nicht allen Einsatzbereichen gewachsen. Insbesondere, wenn die Elektrobleche stark korrosiven Medien wie z. B. Sauergas (hoher Schwefelwasserstoffgehalt) ausgesetzt werden, sind diese Elektrobleche stark korrosionsgefährdet.However, as has been shown, the electrical steel sheets and their coatings available in the above-mentioned standards can not cope with all fields of application. In particular, if the electric sheets strongly corrosive media such. B. acid gas (high hydrogen sulfide content) are exposed, these electrical sheets are highly susceptible to corrosion.

Gemäß der GB 852,265 A können Aluminiumschichten auf Bauteilen aus Eisenlegierungen verwendet werden, um den Stickstoffgehalt in dem Bauteil zu verringern. Dabei bildet sich zwischen der Aluminiumschicht und dem Bauteil eine Zwischenschicht aus Aluminiumnitrid, wobei diese außerdem als Diffusionssperrschicht wirkt, so dass Aluminium nicht in das Bauteil diffundieren kann. Anstelle von Aluminium können auch andere Metalle verwendet werden, welche in der Lage sind, Nitride mit Stickstoff auszubilden. Als Beispiele für solche Metalle werden unter anderem Titan und Tantal genannt.According to the GB 852,265 A For example, aluminum layers on ferroalloy components may be used to reduce the nitrogen content in the component. In this case, an intermediate layer of aluminum nitride is formed between the aluminum layer and the component, which also acts as a diffusion barrier layer, so that aluminum can not diffuse into the component. Instead of aluminum, it is also possible to use other metals which are capable of forming nitrides with nitrogen. Examples of such metals include titanium and tantalum.

Die Aufgabe der Erfindung besteht daher darin, ein Elektroblech anzugeben, welches auch für den Einsatz unter starken korrosiven Bedingungen geeignet ist.The object of the invention is therefore to provide an electrical sheet which is also suitable for use under severe corrosive conditions.

Diese Aufgabe wird mit dem eingangs angegebenen Elektroblech erfindungsgemäß dadurch gelöst, dass die Schicht aus einem Metalloxid, enthaltend hauptsächlich Titanoxid oder Tantaloxid, besteht und dass das Elektroblech eine Diffusionszone aufweist, in die das Metall des Metalloxids in den Werkstoff des Elektrobleches eindiffundiert ist und die an die Schicht angrenzt. Dadurch, dass die Oxidschicht an eine Diffusionsschicht angrenzt, wird vorteilhaft die Haftung der Oxidschicht stark verbessert. Die Verwendung der Metalle, Titan oder Tantal führt dazu, dass die spontan an der Oberfläche des Elektroblechs ausbildende Oxidschicht sehr beständig gegen korrosive Medien ist. Dadurch wird auch ein Einsatz unter extremen korrosiven Bedingungen wie z. B. Sauergas möglich. Es können beispielsweise Motorpumpen betrieben werden, welche für die Förderung von Erdgas im Unterseebereich verwendet werden. Hierdurch ergibt sich eine neue Anwendung der Elektrobleche, die einen Einsatz der elektrischen Maschinen unter vorteilhaft günstigen Wartungsbedingungen erlauben. Falls die sich spontan an Luftsauerstoff ausbildenden Oxidschichten zum wirksamen Korrosionsschutz nicht ausreichen, kann die Oxidschicht auch durch eine elektrochemische Behandlung der Oberfläche hergestellt werden (hierzu im Folgenden mehr).This object is achieved with the above-mentioned electric sheet according to the invention that the layer of a metal oxide containing mainly titanium oxide or tantalum oxide, and that the electrical steel has a diffusion zone in which the metal of the metal oxide is diffused into the material of the electric sheet and the the layer adjoins. Due to the fact that the oxide layer adjoins a diffusion layer, the adhesion of the oxide layer is advantageously greatly improved. The use of metals, titanium or tantalum causes the spontaneously forming on the surface of the electrical sheet oxide layer is very resistant to corrosive media. This also makes use under extreme corrosive conditions such. B. sour gas possible. For example, motor pumps can be operated, which are used for the promotion of natural gas in the subsea area. This results in a new application of the electrical steel sheets, which allow use of electrical machines under favorable favorable maintenance conditions. If the oxide layers forming spontaneously on atmospheric oxygen are not sufficient for effective corrosion protection, the oxide layer can also be produced by an electrochemical treatment of the surface (more on this in the following).

Die sich an die Oxidschicht anschließende Diffusionszone hat zwei Vorteile. Zum einen verbessert die Diffusionszone die Haftung der Oxidschicht, da sich der Übergang zwischen der Oxidschicht und dem Matrixmaterial des Elektroblechs, einer Stahllegierung, kontinuierlich vollzieht, was die Ausbildung von Spannungen vermindert. Außerdem ist es vorteilhaft möglich, dass im Falle von Verletzungen der Oxidschicht das in der Diffusionsschicht befindliche Material an Titan oder Tantal zur Passivierung der Schadstelle herangezogen werden kann. Hierzu diffundiert das betreffende Metall an die Oberfläche, wo eine erneute Passivierung stattfindet. Der Korrosionsschutz bleibt dadurch vorteilhaft erhalten.The diffusion zone following the oxide layer has two advantages. On the one hand, the diffusion zone improves the adhesion of the oxide layer, since the transition between the oxide layer and the matrix material of the electrical steel, a steel alloy, takes place continuously, which reduces the formation of stresses. In addition, it is advantageously possible that in case of damage to the oxide layer, the material contained in the diffusion layer of titanium or tantalum can be used to passivate the damaged area. For this purpose, the metal in question diffuses to the surface, where a renewed passivation takes place. The corrosion protection is thereby advantageously retained.

Gemäß einer Ausgestaltung der Erfindung ist vorgesehen, dass die Schicht eine Dicke von mindestens 5 und höchstens 10 µm aufweist. Hierbei handelt es sich um Schichtdicken der Oxidschicht, die einen wirksamen Korrosionsschutz ermöglichen und in ihrer Herstellung aufgrund der geringen Dicke vorteilhaft einen geringen Fertigungsaufwand und geringen Materialeinsatz erfordern.According to one embodiment of the invention it is provided that the layer has a thickness of at least 5 and at most 10 microns. These are layer thicknesses of the oxide layer, which allow effective corrosion protection and in their production due to the small thickness advantageously require low production costs and low material usage.

Gemäß einer anderen Ausgestaltung der Erfindung ist vorgesehen, dass die Diffusionszone innerhalb eines Abstandes von 2 µm von der Grenzfläche zur Schicht einen Gehalt an Titan oder Tantal von mehr als 50 Gew-% aufweist. Hierbei handelt es sich um Legierungsgehalte, die einen diffusionsbedingten Transport von Titan bzw. Tantal an Schadstellen (wie bereits beschrieben) vorteilhaft noch ermöglichen. Dabei können direkt unterhalb der Oxidschicht auch Gehalte von bis zu 100 % an Titan oder Tantal auftreten. Mit steigendem Abstand von der Oberfläche des Elektrobleches verringert sich der Gehalt an Titan oder Tantal in der Matrix des Elektrobleches (legierter Stahl) so dass der die Haftung der Oxidschicht verbessernde Effekt ausgenutzt werden kann.According to another embodiment of the invention, it is provided that the diffusion zone within a distance of 2 microns from the interface to the layer has a content of titanium or tantalum of more than 50% by weight. These are alloy contents which advantageously permit diffusion-induced transport of titanium or tantalum to damaged areas (as already described). In this case, contents of up to 100% of titanium or tantalum can also occur directly below the oxide layer. As the distance from the surface of the electrical steel increases, the content of titanium or tantalum in the matrix of the electrical steel (alloyed) decreases Steel) so that the adhesion of the oxide layer improving effect can be exploited.

Weiterhin betrifft die Erfindung ein Verfahren zum Behandeln eines Elektrobleches, bei dem das Elektroblech mit einer die elektrische Isolation verbessernden Schicht beschichtet wird. Auf den Stand der Technik ist bereits eingegangen worden. Die Aufgabe, die sich davon ausgehend ergibt, liegt darin, ein Verfahren anzugeben, mit dem das Behandeln von Elektroblechen möglich ist und welches Produkte erzeugt, die auch unter stark korrosiven Einflüssen einen genügenden Korrosionsschutz gewährleisten.Furthermore, the invention relates to a method for treating an electric sheet, in which the electrical sheet is coated with an electrical insulation improving layer. The prior art has already been discussed. The task which results from this is to specify a method with which the treatment of electrical steel sheets is possible and which produces products which ensure sufficient corrosion protection even under strongly corrosive influences.

Diese Aufgabe wird mit dem genannten Verfahren erfindungsgemäß dadurch gelöst, dass in einem ersten Schritt eine Diffusionszone an der Oberfläche des Elektrobleches hergestellt wird, wobei als Metall Tantal oder Titan in die Oberfläche eindiffundiert, wobei der erste Schritt als PVD-Prozess in einer inerten Gasatmosphäre mit einer nachfolgenden Wärmebehandlung durchgeführt wird. In einem zweiten Schritt wird das Metall, Tantal oder Titan an der Oberfläche in das zugehörige Metalloxid, Titanoxid oder Tantaloxid umgewandelt, wobei eine Schicht aus dem Metalloxid entsteht und in der Diffusionszone ein Restgehalt an dem Metall des Metalloxids verbleibt. Hierdurch entsteht die bereits oben erläuterte Oxidschicht, die einen hervorragenden Widerstand gegen Korrosion aufweist. In der Diffusionszone verbleibt der Restgehalt an dem Metall des Metalloxides, wodurch, wie bereits erläutert, die Haftung der Oxidschicht verbessert wird. Außerdem entsteht durch die Diffusionszone ein Depot an dem entsprechenden Material, welches bei Verletzungen der Oxidschicht zum Ausheilen der Verletzung durch spontanes Passivieren zur Verfügung steht.This object is achieved with the mentioned method according to the invention in that in a first step, a diffusion zone is produced on the surface of the electric sheet, wherein as a metal tantalum or titanium diffused into the surface, wherein the first step as a PVD process in an inert gas atmosphere a subsequent heat treatment is performed. In a second step, the metal, tantalum or titanium on the surface is converted into the associated metal oxide, titanium oxide or tantalum oxide, wherein a layer of the metal oxide is formed and remains in the diffusion zone, a residual content of the metal of the metal oxide. This results in the already discussed above oxide layer, which has excellent resistance to corrosion. In the diffusion zone, the residual content remains on the metal of the metal oxide, whereby, as already explained, the adhesion of the oxide layer is improved. In addition, a depot is formed by the diffusion zone on the corresponding material, which is available in case of injuries of the oxide layer to heal the injury by spontaneous passivation.

Das genannte Verfahren wird so durchgeführt, dass der erste Schritt als PVD-Prozess mit einer nachfolgenden Wärmebehandlung durchgeführt wird. PVD-Prozesse sind vorteilhaft leicht zu handhaben. Sowohl Titan als auch Tantal lassen sich durch Verwendung geeigneter Targetmaterialien auf Stahl abscheiden. Titan wird beispielsweise zur Herstellung von Werkzeugbeschichtungen in vielfacher Weise durch PVD-Verfahren abgeschieden, wobei dies normalerweise in einer reaktiven Stickstoffatmoshäre erfolgt, um Titannitrid herstellen zu können. Wird stattdessen eine inerte Gasatmosphäre gewählt, so wird reines Titan abgeschieden. Auch Tantal lässt sich ohne weiteres auf Stahl abscheiden. Ein derartiges Verfahren ist beispielsweise in der EP 77 535 A1 beschrieben. Die Abscheidung von Titan kann beispielsweise auch durch Spraying oder Pulverbeschichten erfolgen, wie beispielsweise dem Derwent Abstract mit der Accession Number 1978-43006 A (korrespondierend zu JP 53-50019 A ) zu entnehmen ist. Die Pulverprozesse werden auch als Packprozesse bezeichnet, wobei hierbei die Diffusionsschichten durch ein Diffundieren des Tantals in das Werkstück entstehen. Anders als bei PVD-Prozessen entsteht damit die Diffusionsschicht sofort, während bei PVD-Prozessen nach dem Beschichtungsvorgang eine Wärmebehandlung erfolgen muss, die zu einem Eindiffundieren des Tantals oder des Titans in die Matrix des Elektroblechs führt. Parameter für derartige Diffusionsbehandlungen sind allgemein bekannt und lassen sich beispielsweise dem Derwent Abstract mit der Accession Number 1984-104398 (korrespondierend zu JP 59-47371 A ) entnehmen. Neben den oben genannten Behandlungsmethoden sind grundsätzlich auch elektrochemische Beschichtungen beispielsweise in einem Salzbad denkbar oder auch ein Beschichten mittels CVD.Said method is performed such that the first step is performed as a PVD process with a subsequent heat treatment. PVD processes are advantageously easy to handle. Both titanium and tantalum can be deposited on steel by using suitable target materials. For example, titanium is deposited in multiple ways by PVD processes to make tool coatings, usually in a reactive nitrogen atmosphere, to produce titanium nitride. If instead an inert gas atmosphere is selected, pure titanium is deposited. Tantalum can also be easily deposited on steel. Such a method is for example in the EP 77 535 A1 described. The deposition of titanium, for example, by spraying or powder coating done, such as the Derwent Abstract with the Accession Number 1978-43006 A (corresponding to JP 53-50019 A ) can be seen. The powder processes are also referred to as packing processes, in which case the diffusion layers are formed by diffusing the tantalum into the workpiece. In contrast to PVD processes, the diffusion layer thus arises immediately, whereas in PVD processes after the coating process, a heat treatment has to take place, which leads to an inward diffusion of the tantalum or titanium into the matrix of the electrical sheet. Parameters for such diffusion treatments are well known and can be found, for example, in the Derwent Abstract with the Accession Number 1984-104398 (corresponding to US Pat JP 59-47371 A ) remove. In addition to the abovementioned treatment methods, electrochemical coatings, for example in a salt bath, are also conceivable in principle, or else coating by means of CVD.

Gemäß einer Ausgestaltung des erfindungsgemäßen Verfahrens ist vorgesehen, dass die Diffusionszone vor der Ausbildung der Schicht innerhalb eines Abstandes von 5 µm von der Grenzfläche zur Schicht einen Gehalt an Titan oder Tantal von mehr als 50 Gew-% aufweist. Es ist selbstverständlich, dass die Diffusionszone vor der Ausbildung der Schicht einen größeren Bereich mit einer hohen Titan- oder Tantal-Konzentration aufweisen muss, da durch Oxidation des Titans oder Tantals ein Teil der vorher ausgebildeten Diffusionsschicht in die Oxidschicht umgewandelt wird. Um nach diesem Oxidationsvorgang noch genügend Material für ein Reparieren der Oxidschicht in der Matrix des Elektrobleches zur Verfügung zu haben, muss daher der Anteil an Titan oder Tantal genügend hoch sein.According to one embodiment of the method according to the invention, it is provided that the diffusion zone before the formation of the layer within a distance of 5 microns from the interface to the layer has a content of titanium or tantalum of more than 50% by weight. It goes without saying that the diffusion zone must have a larger area with a high titanium or tantalum concentration before the formation of the layer, since a portion of the previously formed diffusion layer is converted into the oxide layer by oxidation of the titanium or tantalum. In order to still have enough material for a repair of the oxide layer in the matrix of the electrical steel available after this oxidation process, therefore, the proportion of titanium or tantalum must be sufficiently high.

Für den Fall, dass eine spontan sich ausbildende Passivierungsschicht auf dem Titan oder dem Tantal für einen wirksamen Korrosionsschutz nicht ausreicht, sondern die Passivierungsschicht elektrochemisch hergestellt werden soll, ist es vorteilhaft, eine sich spontan ausbildende Passivierungsschicht vorher zu entfernen. Auf diese Weise kann vorteilhaft die elektrochemisch unterstützte Ausbildung der Passivierungsschicht ungestört erfolgen. Die Wärmebehandlung findet dann vorteilhaft in einer sauerstoffhaltigen Atmosphäre statt, wobei bevorzugt der Sauerstoff im Vergleich zur atmosphärischen Bedingungen auch angereichert sein kann, um den Oxidationsvorgang zu beschleunigen.In the event that a spontaneously forming passivation layer on the titanium or the tantalum is not sufficient for effective corrosion protection, but the passivation layer is to be produced electrochemically, it is advantageous to previously remove a spontaneously forming passivation layer. In this way, advantageously the electrochemically assisted formation of the passivation layer can take place undisturbed. The heat treatment then advantageously takes place in an oxygen-containing atmosphere, wherein preferably the oxygen can also be enriched in comparison to the atmospheric conditions in order to accelerate the oxidation process.

Weitere Einzelheiten der Erfindung werden nachfolgend anhand der Zeichnung beschrieben. Die einzige Figur zeigt ein Ausführungsbeispiel des erfindungsgemäßen Elektrobleches im Querschnitt. Zu erkennen ist in der Figur ein Elektroblech 11, dessen Oberseite 12 und Unterseite 13 jeweils mit einer Schicht 14 aus Tantaloxid versehen ist. Dieser Schicht 14 schließt sich eine Diffusionszone 15 an, die eine gemeinsame Grenzfläche 16 mit der Schicht 12 des Tantaloxids aufweist. Hinter der Grenzfläche liegt die Konzentration an Tantal in der Diffusionszone weit über 50 %. Diese fällt zum Inneren des Elektrobleches 11 immer weiter ab, bis die Konzentration 0 Gew-% beträgt. An sich lässt sich daher eine Grenze zwischen dem eigentlichen Elektroblech 11 und der Diffusionszone 15 nicht wirklich darstellen. In der Figur dargestellt ist jedoch derjenige Bereich, in dem die Konzentration an Tantal im Gefüge des Elektrobleches 11 über 50 % liegt.Further details of the invention are described below with reference to the drawing. The single FIGURE shows an embodiment of the electric sheet metal according to the invention in cross section. Evident is in the figure, an electric sheet 11, the top 12 and bottom 13 is provided in each case with a layer 14 of tantalum oxide. This layer 14 is followed by a diffusion zone 15, which has a common interface 16 with the layer 12 of tantalum oxide. Behind the interface, the concentration of tantalum in the diffusion zone is well over 50%. This falls to the interior of the electric sheet 11 continues until the concentration is 0% by weight. In itself, therefore, a boundary between the actual electrical sheet 11 and the diffusion zone 15 can not really represent. However, the figure shows the region in which the concentration of tantalum in the microstructure of the electrical sheet 11 is more than 50%.

Claims (7)

  1. Magnetic steel sheet (11) having a layer (14) which improves the electrical insulation,
    characterized
    in that the layer (14) consists of a metal oxide containing mainly titanium oxide or tantalum oxide, and in that the magnetic steel sheet (11) has a diffusion zone (15), into which the metal of the metal oxide has diffused into the material of the magnetic steel sheet and which adjoins the layer (14).
  2. Magnetic steel sheet according to Claim 1,
    characterized
    in that the layer (14) has a thickness of at least 5 µm and at most 10 µm.
  3. Magnetic steel sheet according to Claim 1 or 2,
    characterized
    in that the diffusion zone (15) has a titanium or tantalum content of more than 50% by weight within a distance of 2 µm from the interface with the layer (14).
  4. Method for treating a magnetic steel sheet, in which method the magnetic steel sheet (11) is coated with a layer (14) which improves the electrical insulation,
    characterized in that
    - in a first step, a diffusion zone (15) is produced on the surface of the magnetic steel sheet (11), tantalum or titanium diffusing as metal into the surface, the first step being carried out as a PVD process in an inert gas atmosphere with a subsequent heat treatment; and
    - in a second step, the tantalum or titanium metal at the surface is converted into the associated metal oxide, titanium oxide or tantalum oxide, a layer (14) consisting of the metal oxide being formed and a residual content of the metal of the metal oxide remaining in the diffusion zone (15).
  5. Method according to Claim 4,
    characterized
    in that, before the formation of the layer, the diffusion zone (15) has a titanium or tantalum content of more than 50% by weight within a distance of 5 µm from the interface with the layer (14).
  6. Method according to either of Claims 4 and 5,
    characterized
    in that a spontaneously formed passivation layer is removed before the second step is carried out.
  7. Method according to one of Claims 4 to 6,
    characterized
    in that the second step is carried out as a heat treatment in an oxygen-containing atmosphere.
EP14721254.2A 2013-05-10 2014-04-17 Electrical steel sheet with a coating improving the electrical insulation and method of its manufacture Active EP2979281B1 (en)

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DE102013208617.2A DE102013208617A1 (en) 2013-05-10 2013-05-10 Electrical sheet with an electrical insulation improving layer and method for its production
PCT/EP2014/057879 WO2014180646A1 (en) 2013-05-10 2014-04-17 Electrical steel sheet with a layer improving the electrical insulation and method for the production thereof

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KR102176346B1 (en) * 2018-11-30 2020-11-09 주식회사 포스코 Electrical steel sheet and manufacturing method of the same
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CA2911552C (en) 2017-12-05

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