EP0752012B1 - Procede de production de toles electromagnetiques a enrobage verre - Google Patents

Procede de production de toles electromagnetiques a enrobage verre Download PDF

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Publication number
EP0752012B1
EP0752012B1 EP95912252A EP95912252A EP0752012B1 EP 0752012 B1 EP0752012 B1 EP 0752012B1 EP 95912252 A EP95912252 A EP 95912252A EP 95912252 A EP95912252 A EP 95912252A EP 0752012 B1 EP0752012 B1 EP 0752012B1
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EP
European Patent Office
Prior art keywords
annealing separator
additive
mgo
strip
annealing
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.)
Expired - Lifetime
Application number
EP95912252A
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German (de)
English (en)
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EP0752012A1 (fr
Inventor
Fritz Bölling
Brigitte Hammer
Thomas Dolle
Klaus Gehnen
Heiner Schrapers
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
EBG Gesellschaft fuer Elektromagnetische Werkstoffe
Original Assignee
EBG Gesellschaft fuer Elektromagnetische Werkstoffe
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Publication of EP0752012A1 publication Critical patent/EP0752012A1/fr
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    • 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
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • 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
    • C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D5/00—Coating with enamels or vitreous layers
    • C23D5/02—Coating with enamels or vitreous layers by wet methods
    • 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

Definitions

  • the invention relates to a method for producing Electrical sheets, especially grain-oriented ones Electrical sheets, with an evenly adhering Glass film and with improved magnetic properties, in which the hot strip initially produced and possibly annealed except for the final cold strip thickness with at least one Cold rolling stage is cold rolled, then to the an annealing separator rolled to the final thickness is applied and dried and then the cold-rolled strip coated in a high-temperature annealing is subjected, with an integral part of the Glow separator an aqueous magnesium oxide (MgO) dispersion and the glow separator is additionally at least one Has additive.
  • MgO aqueous magnesium oxide
  • decarburization annealing is carried out after rolling to the final thickness.
  • the carbon is extracted from the material.
  • An oxide layer forms as a base layer on the strip surface, the essential components of which are silicon dioxide (SiO 2 ) and fayalite (Fe 2 SiO 4 ).
  • the strip is coated with a protective layer and subjected to a long-term annealing in the coil.
  • the adhesive protection layer is intended to prevent the individual coil turns from sticking together during long-term annealing and, on the other hand, to form an insulation layer (glass film) with the base layer on the strip surface.
  • the adhesive protection layer consists essentially of magnesium oxide (MgO).
  • the MgO is slurried in water in the form of a powder, applied to the belt and dried. During this process, part of the magnesium oxide reacts with the water to form magnesium hydroxide (Mg (OH) 2 ). The amount of water bound to magnesium hydroxide, based on the total amount of oxide powder, is called the loss on ignition.
  • Equation (I) shows the dehydration of the magnesium hydroxide, which starts at about 350 ° C. It is important for an optimally running process, both in terms of the insulation and the development of the magnetic properties, that the amount of water released is within certain limits.
  • the water humidifies the predominantly hydrogen-containing annealing atmosphere and thus sets a corresponding oxidation potential.
  • the annealing atmosphere must not be too dry because the glass film would be made too thin under such conditions. However, it must also not become too moist, because then it will be reoxidized too much and the glass film will have defects such as local flaking and poor adhesion.
  • additives to MgO powder were introduced to improve the formation of the insulation layer and the magnetic properties of the finished product.
  • These include titanium dioxide (TiO 2 ), boron compounds such as boron oxide (B 2 O 3 ) or sodium tetraborate (Na 2 B 4 O 7 ), as well as antimony compounds such as antimony sulfate (Sb 2 (SO 4 ) 3 ) in combination with a chloride, preferably antimony chloride SbCl 3 .
  • TiO 2 titanium dioxide
  • boron compounds such as boron oxide (B 2 O 3 ) or sodium tetraborate (Na 2 B 4 O 7 )
  • antimony compounds such as antimony sulfate (Sb 2 (SO 4 ) 3 ) in combination with a chloride, preferably antimony chloride SbCl 3 .
  • the additives used often also have disadvantages that reduce the product quality. Overall, the processing of such additives is cumbersome, since some of them have to be dissolved in previously
  • the invention is based on the object of measures to meet, especially by modifying the Glow separators to the insulation properties and at the same time the magnetic properties of the Finished product to improve further.
  • the Anti-adhesive layer can be applied more homogeneously quality-reducing phenomena, such as glow contours and to avoid local defects.
  • one should easy handling can be guaranteed and the cost, am Standard measured, kept low.
  • a readily water-soluble one Sodium phosphate compound is used.
  • a readily water soluble sodium phosphate compound and a finely dispersed oxidic aluminum compound Glow separator can be added.
  • the good water solubility of the sodium phosphate compound if necessary in combination with the finely dispersed distribution of the oxidic aluminum compound in the specified amounts ensure a homogeneous application of the adhesive protection, prevent coagulation within the aqueous Magnesium oxide dispersion and associated local Defects in the glass film and promote those in the Long-term annealing chemical reactions between the one on the belt surface Base layer and the adhesive protective layer to the glass film.
  • a stronger than the standard Glass film formation that the interaction between the Annealing atmosphere and the strips are positively influenced the magnetic properties of the electrical sheets improved.
  • a method with the generic measures has been known from EP 0 232 537 B1.
  • a titanium compound such as TiO 2
  • a boron compound such as B 2 O 3
  • a sulfur compound such as SrS
  • the MgO-based annealing separator is added to the MgO-based annealing separator as an additive, with the aim of improving the insulation properties, such as Adhesion and the appearance of the glass film to influence positively. This is achieved by hydrating the coating.
  • the magnetic properties were also improved by the addition of such additives.
  • JP-5-513 8021 describes a release agent based on MgO, which contains up to 50% by weight of Mg (OH) 2 and up to 5% by weight of Al (OH) 3 or Al (NO 3 ) 3 contains. It has been shown that the use of such a release agent for coating electrical sheets does not have an adverse effect on the magnetic properties of the product.
  • JP-5-247 661 describes a process for the production of grain-oriented silicon steels which are coated with a glass layer.
  • improvements in the magnetic properties and the surface properties of the coated steel are achieved by using release agent additives such as Sb 2 (SO 4 ) 3 , V 2 O s , SrS, Na 2 B 4 O 7 and Ca (H 2 PO 4 ) 2 .
  • the positive influence on which the invention is based the magnetic properties is characteristic of the sodium phosphates.
  • FIG. 1 shows the superiority of the samples produced by the method according to the invention with an MgO-based adhesive protection doped with sodium phosphate over other phosphate additives.
  • HGO high permeability grain oriented tape samples were coated with MgO + 6% TiO 2 + the listed additives, dried and annealed.
  • the sodium phosphates are readily water-soluble, allow thus an optimally homogeneous distribution within the Anti-adhesive layer.
  • Sodium phosphates in the present case in particular using the example of Sodium pyrophosphate decahydrate are reported both the magnetic properties polarization and Magnetic loss, as well Isolation training improved.
  • the Inhibitor test method is demonstrated that the Sodium pyrophosphate to a prematurely stronger one Glass film formation leads.
  • the inhibitor test stops Process in which, in principle, high annealing certain annealing temperatures are canceled and the Samples can be assessed magnetically. In the present case the insulation training was also assessed.
  • the magnetic properties of loss of magnetization P 1.7 and polarization J 800 were determined on the annealed strips.
  • the aluminum compounds used as a further additive in addition to the sodium phosphate compound are aluminum oxides or hydroxides of the form Al 2 O 3 , AlO (OH) 3 and AL (OH), the effect of which is fully exploited when the corresponding particle sizes are small. The effect is particularly evident when the compounds are added in the form of sols (very fine particles / water mixtures).
  • the average particle size should be less than 100 nm with the narrowest possible particle size distribution.
  • the addition of these aluminum compounds leads to a considerable improvement in loss, similar to the case with the addition of titanium dioxide.
  • the advantage of the aluminum compound as an additive over titanium dioxide is the lower dosage and the more homogeneous distribution of the particles. Another advantage lies in the fact that the aluminum compounds added also have the property of a ceramic binder, and the adhesive protective layer therefore adheres better to the tape.
  • Table 6 and Figure 3 show the influence of the selected aluminum compounds on the magnetic loss. Influence of different oxidic aluminum compounds on the magnetic properties and the glass film appearance
  • Boehmite AIO (OH) 0 0.5 2nd Glass film appearance
  • the effect of the above additives is optimized, if suitable combinations of additives are used. This also has positive effects in combination with additives already used, such as titanium dioxide, Antimony sulfate and sodium tetraborate achieved. Related to the slurry properties and thus the homogeneity of the MgO layer turns out to be a combination of one finely dispersed oxidic aluminum compound and one well water-soluble sodium phosphate as optimal because with these additives significantly fewer local defects to be observed.
  • the magnetic properties of loss of magnetization P 1.7 and polarization J 800 were determined on the annealed strips.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Power Engineering (AREA)
  • Electromagnetism (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Insulating Bodies (AREA)
  • Inorganic Insulating Materials (AREA)
  • Glass Compositions (AREA)
  • Laminated Bodies (AREA)
  • Cell Separators (AREA)

Claims (7)

  1. Procédé de production de tôles électriques, en particulier de tôles électriques à grain orienté munies d'un film vitreux uniforme et bien adhérent et possédant des propriétés magnétiques améliorées, dans lequel la bande chaude initialement produite et éventuellement recuite est laminée à froid à l'épaisseur finale de la bande à froid, par au moins un étage de laminage à froid, un séparateur de recuit est déposé et séché ensuite sur la bande laminée à l'épaisseur finale, à la suite de quoi la bande à froid ainsi revêtue est soumise à un recuit à haute température, dans lequel une partie constitutive essentielle du séparateur de recuit est une dispersion aqueuse d'oxyde de magnésium (MgO) et le séparateur de recuit contient en supplément au moins un additif
       caractérisé en ce qu'on utilise comme au moins un additif, un composé de phosphate de sodium bien soluble dans l'eau.
  2. Procédé selon la revendication 1,
       caractérisé en ce qu'on utilise au moins deux additifs, à savoir un composé de phosphate de sodium bien soluble dans l'eau et un composé d'aluminium oxydé finement dispersé.
  3. Procédé selon la revendication 1 ou 2,
       caractérisé en ce qu'on ajoute comme additif au séparateur de recuit 0,05 à 4,0 % de phosphate de sodium, rapporté à la quantité de MgO.
  4. Procédé selon la revendication 1 ou 2,
       caractérisé en ce qu'on ajoute comme additif au séparateur de recuit 0,3 à 1,5 % de pyrophosphate de sodium décahydraté, rapporté à la quantité de MgO.
  5. Procédé selon la revendication 2, 3 ou 4,
       caractérisé en ce qu'on ajoute comme additif au séparateur de recuit 0,05 à 4,0 % du composé d'aluminium oxydé finement dispersé, rapporté à la quantité de MgO.
  6. Procédé selon la revendication 2, 3, 4 ou 5,
       caractérisé en qu'on utilise le composé d'aluminium oxydé dans une dimension de particules inférieure à 100 nm.
  7. Procédé selon une des revendications 1 à 6,
       caractérisé en ce qu'on ajoute au séparateur de recuit d'autres additifs tels que l'oxyde de titane, l'oxyde de bore, le tétraborate de sodium, le sulfate d'antimoine, un chlorure métallique, de préférence le chlorure d'antimoine.
EP95912252A 1994-03-22 1995-03-18 Procede de production de toles electromagnetiques a enrobage verre Expired - Lifetime EP0752012B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4409691 1994-03-22
DE4409691A DE4409691A1 (de) 1994-03-22 1994-03-22 Verfahren zur Herstellung von Elektroblechen mit einem Glasüberzug
PCT/EP1995/001020 WO1995025820A1 (fr) 1994-03-22 1995-03-18 Procede de production de toles electromagnetiques a enrobage verre

Publications (2)

Publication Number Publication Date
EP0752012A1 EP0752012A1 (fr) 1997-01-08
EP0752012B1 true EP0752012B1 (fr) 1998-08-26

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EP95912252A Expired - Lifetime EP0752012B1 (fr) 1994-03-22 1995-03-18 Procede de production de toles electromagnetiques a enrobage verre

Country Status (10)

Country Link
US (1) US5863356A (fr)
EP (1) EP0752012B1 (fr)
JP (1) JP3730254B2 (fr)
KR (1) KR100367985B1 (fr)
AT (1) ATE170226T1 (fr)
CZ (1) CZ292216B6 (fr)
DE (2) DE4409691A1 (fr)
PL (1) PL178890B1 (fr)
RU (1) RU2139945C1 (fr)
WO (1) WO1995025820A1 (fr)

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JP3475258B2 (ja) * 1994-05-23 2003-12-08 株式会社海水化学研究所 セラミック被膜形成剤およびその製造方法
DE19750066C1 (de) * 1997-11-12 1999-08-05 Ebg Elektromagnet Werkstoffe Verfahren zum Beschichten von Elektrostahlbändern mit einem Glühseparator
DE102004014596A1 (de) * 2004-03-23 2005-10-27 Trithor Gmbh Antihaftbeschichtung für die Herstellung von Kompositwerkstoff-Drähten
JP5633178B2 (ja) * 2010-04-27 2014-12-03 Ｊｆｅスチール株式会社 方向性電磁鋼板用焼鈍分離剤
DE102010038038A1 (de) * 2010-10-07 2012-04-12 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Erzeugen einer Isolationsbeschichtung auf einem kornorientierten Elektro-Stahlflachprodukt und mit einer solchen Isolationsbeschichtung beschichtetes Elektro-Stahlflachprodukt
CN102453793B (zh) * 2010-10-25 2013-09-25 宝山钢铁股份有限公司 用于具有优良磁性能的镜面取向硅钢制备的退火隔离剂
WO2012096350A1 (fr) * 2011-01-12 2012-07-19 新日本製鐵株式会社 Tôle d'acier magnétique à grains orientés et processus de fabrication de celle-ci
JP5360272B2 (ja) * 2011-08-18 2013-12-04 Ｊｆｅスチール株式会社 方向性電磁鋼板の製造方法
IN2014MN00456A (fr) * 2011-10-04 2015-06-19 Jfe Steel Corp
DE102015114358B4 (de) 2015-08-28 2017-04-13 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten Elektrobands und kornorientiertes Elektroband
KR101909218B1 (ko) * 2016-12-21 2018-10-17 주식회사 포스코 방향성 전기강판용 소둔 분리제 조성물, 방향성 전기강판 및 방향성 전기강판의 제조방법
JP6939767B2 (ja) * 2018-12-27 2021-09-22 Ｊｆｅスチール株式会社 方向性電磁鋼板用焼鈍分離剤および方向性電磁鋼板の製造方法
JP6939766B2 (ja) * 2018-12-27 2021-09-22 Ｊｆｅスチール株式会社 方向性電磁鋼板用焼鈍分離剤および方向性電磁鋼板の製造方法
CN111906142B (zh) * 2020-06-24 2022-08-16 浙江博星工贸有限公司 一种控制冷轧不锈钢带力学性能的工艺
CN114014529B (zh) * 2021-12-17 2023-02-21 中国建筑材料科学研究总院有限公司 一种硼硅酸盐玻璃珠火抛用的隔离剂
CN114854960B (zh) * 2022-03-30 2023-09-05 武汉钢铁有限公司 一种减少取向硅钢表面缺陷的退火隔离剂及其使用方法

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Also Published As

Publication number Publication date
KR970701795A (ko) 1997-04-12
EP0752012A1 (fr) 1997-01-08
PL178890B1 (pl) 2000-06-30
PL316139A1 (en) 1996-12-23
WO1995025820A1 (fr) 1995-09-28
DE59503345D1 (de) 1998-10-01
RU2139945C1 (ru) 1999-10-20
KR100367985B1 (ko) 2003-08-02
US5863356A (en) 1999-01-26
DE4409691A1 (de) 1995-09-28
JPH09510503A (ja) 1997-10-21
CZ292216B6 (cs) 2003-08-13
JP3730254B2 (ja) 2005-12-21
ATE170226T1 (de) 1998-09-15
CZ273896A3 (en) 1997-04-16

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