KR100600805B1 - A method for manufacturing annealing separator of oriented electrical steel sheet - Google Patents

A method for manufacturing annealing separator of oriented electrical steel sheet Download PDF

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KR100600805B1
KR100600805B1 KR1020050034037A KR20050034037A KR100600805B1 KR 100600805 B1 KR100600805 B1 KR 100600805B1 KR 1020050034037 A KR1020050034037 A KR 1020050034037A KR 20050034037 A KR20050034037 A KR 20050034037A KR 100600805 B1 KR100600805 B1 KR 100600805B1
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magnesium oxide
steel sheet
electrical steel
magnesium
annealing separator
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손동환
김병수
김동한
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주식회사 포스렉
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C20/00Chemical coating by decomposition of either solid compounds or suspensions of the coating forming compounds, without leaving reaction products of surface material in the coating
    • C23C20/06Coating with inorganic material, other than metallic material
    • C23C20/08Coating with inorganic material, other than metallic material with compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/02Magnesia
    • C01F5/06Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • 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

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)

Abstract

본 발명은 방향성 전기강판용 소둔분리제의 제조방법에 관한 것이다.The present invention relates to a method for producing an annealing separator for grain-oriented electrical steel sheet.

본 발명은 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 700~900℃로 소성하여 산화마그네슘(산화마그네슘A)을 제조하는 단계; 해수 또는 간수와 석회를 반응시켜 생성된 수산화마그네슘을 1000~1200℃로 소성하여 산화마그네슘(산화마그네슘B)을 제조하는 단계; 및 상기 산화마그네슘A: 35~45중량% 및 상기 산화마그네슘B: 55~65중량%를 혼합하는 단계;를 포함하는 방향성 전기강판용 소둔분리제의 제조방법에 관한 것이다.The present invention is to prepare a magnesium oxide (magnesium oxide A) by calcining the magnesium hydroxide produced by reacting magnesium chloride and caustic soda at 700 ~ 900 ℃; Preparing magnesium oxide (magnesium oxide B) by calcining magnesium hydroxide produced by reacting seawater or brine with lime at 1000 to 1200 ° C; And a step of mixing the magnesium oxide A: 35 to 45 wt% and the magnesium oxide B: 55 to 65 wt%.

본 발명의 방향성 전기강판용 소둔분리제는 균일한 피막특성 및 우수한 자기특성을 갖는 방향성 전기강판의 제조가 가능하게 한다.The annealing separator for grain-oriented electrical steel sheet of the present invention enables the production of grain-oriented electrical steel sheet having uniform coating properties and excellent magnetic properties.

산화마그네슘, 소둔온도, 활성도, 활성마그네시아, TiO2, 붕사, 소둔분리제, 전기강판 Magnesium oxide, annealing temperature, activity, activated magnesium, TiO2, borax, annealing separator, electrical steel sheet

Description

방향성 전기강판용 소둔분리제의 제조방법{A method for manufacturing annealing separator of oriented electrical steel sheet}A method for manufacturing annealing separator of oriented electrical steel sheet}

본 발명은 방향성 전기강판용 소둔분리제의 제조방법에 관한 것으로, 보다 상세하게는 균일한 피막형성 및 우수한 자기특성을 갖는 전기강판을 제조할 수 있는 방향성 전기강판용 소둔분리제의 제조방법에 관한 것이다.The present invention relates to a method for producing an annealing separator for grain-oriented electrical steel sheet, and more particularly, to a method for producing an annealing separator for grain-oriented electrical steel sheet capable of producing an electrical steel sheet having uniform film formation and excellent magnetic properties.

방향성 전기강판은 우수한 자기적 특성을 가지므로 주로 변압기, 발전기 등의 철심재료로 사용된다. 이러한 방향성 전기강판은 2~4중량%의 규소(Si)를 함유하는 규소강을 열연, 냉연, 탈탄소둔 및 마무리소둔함으로써 제조된다. 이때 소둔분리제인 산화마그네슘은 Si와 반응하여 포스테라이트(2MgOㆍSiO2)를 생성함으로써, 고온소둔시 강판의 융착이 생기지 않도록 분리시키는 역할을 하게 된다. 또한, 상기 산화마그네슘은 방향성 전기강판에 절연성, 장력부여성 등을 부여하게 되며, 공정도중 물과의 수화, 과산화, 불균일화로 인하여 피막특성 및 자기특성을 저하시키는 경우가 있으므로 도포되는 산화마그네슘의 특성은 매우 중요하다. 이 경우 강판 의 피막특성 및 자기특성에 영향을 주는 인자로는 산화마그네슘의 활성도, 순도, 입도, 부착성 등이 있으며, 강판에 도포될때는 수화의 진행비율, 입자의 분산상태, 도포량 등이 강판의 피막특성 및 자기특성에 영향을 미치게 된다.Since oriented electrical steel has excellent magnetic properties, it is mainly used as iron core materials of transformers and generators. Such a grain-oriented electrical steel sheet is produced by hot rolling, cold rolling, decarbonization, and finish annealing of silicon steel containing 2 to 4% by weight of silicon (Si). At this time, magnesium oxide, an annealing separator, reacts with Si to generate forsterite (2MgO.SiO 2 ), thereby separating the steel sheet from fusion during hot annealing. In addition, the magnesium oxide imparts insulation, tensile stress, and the like to the grain-oriented electrical steel sheet, and may degrade the coating properties and magnetic properties due to hydration, peroxidation, and non-uniformity with water during the process. Is very important. In this case, factors affecting the film properties and the magnetic properties of the steel sheet include the activity, purity, particle size, and adhesion of magnesium oxide, and when applied to the steel sheet, the progress rate of hydration, the dispersion state of particles, the amount of coating, etc. This will affect the film and magnetic properties of the film.

상기와 같은 전기강판의 소둔분리제에 관한 종래기술로는 대한민국 공개특허공보 1989-9766호와 2004-41774호가 있다. 상기 종래기술들중 대한민국 공개특허공보 1989-9766호의 경우에는 수산화마그네슘을 950~1050℃로 소성한 소둔분리제를 이용하고 있으나, 이러한 소둔분리제는 Si와의 반응율이 낮아 강판표면의 피막형성에 문제가 있다. 또한, 상기 종래기술들중 대한민국 공개특허공보 2004-41774호의 경우에는 MgO분말 100중량%에 Fe-Si계 소성분말을 첨가한 침규확산용 분말도포제를 제시하고 있으나, 이러한 소둔분리제는 MgO의 분산성이 나빠 소둔시 도포량 관리가 어려울 뿐만 아니라 강판위치별 침규량 관리가 어려운 문제점이 있다.Conventional techniques related to annealing separators for electrical steel sheets as described above include Korean Patent Publication Nos. 1989-9766 and 2004-41774. Korean Patent Publication No. 1989-9766 of the prior art uses an annealing separator calcined with magnesium hydroxide at 950 ~ 1050 ℃, but the annealing separator is low in the reaction rate with Si, a problem in forming the film on the surface of the steel sheet There is. In addition, the Republic of Korea Patent Publication No. 2004-41774 of the prior art has proposed a powder coating agent for immersion diffusion to which Fe-Si-based small powder is added to 100% by weight of MgO powder, the annealing separator is powder of MgO It is difficult to manage the coating amount at the time of annealing due to the bad acidity, and it is difficult to manage the deposit amount by steel sheet position.

상기 종래기술 이외에도 반응성 등을 고려하여 수산화마그네슘을 직접 사용하는 기술이 있으나, 이러한 종래기술의 경우에는 마무리소둔중에 다량의 물이 발생되어 자성을 열화시키는 문제점이 있다. 또한, 500~700℃의 저온으로 경소한 산화마그네슘을 이용하는 기술이 있으나, 이러한 종래기술은 시간이 지남에 따라 수화속도가 빨라져 함유 수분량이 증가함으로써 안정적인 자성확보가 어려운 문제점이 있다. 또한, 1200℃ 이상의 고온으로 소성한 산화마그네슘을 이용하는 기술이 있으나, 이러한 종래기술은 포스테라이트의 생성이 어려워 강판표면에 안정적인 피막 형성이 어려운 문제점이 있다.In addition to the prior art, there is a technique of directly using magnesium hydroxide in consideration of reactivity, but in the case of such a prior art, a large amount of water is generated during finishing annealing to deteriorate magnetic properties. In addition, there is a technique using a magnesium oxide light at a low temperature of 500 ~ 700 ℃, this prior art has a problem that it is difficult to secure a stable magnetic as the hydration rate is increased over time to increase the moisture content. In addition, there is a technique of using magnesium oxide calcined at a high temperature of 1200 ℃ or more, this conventional technique is difficult to form a forsterite, there is a problem that it is difficult to form a stable film on the surface of the steel sheet.

본 발명은 상기 종래기술들의 문제점을 해결하기 위한 것으로, 서로 다른 종류의 수산화마그네슘을 각각 그 소성온도를 다르게 제어하여 활성을 제어함으로써 균일한 피막특성을 가질 뿐만 아니라 자기특성도 우수한 전기강판을 제조할 수 있는 방향성 전기강판용 소둔분리제의 제조방법을 제공하는데, 그 목적이 있다.The present invention is to solve the problems of the prior art, and to control the activity by controlling the firing temperature of different types of magnesium hydroxide, respectively, to produce an electrical steel sheet having not only uniform film properties but also excellent magnetic properties. Provided is a method for producing an annealing separator for a grain-oriented electrical steel sheet, the object of which is.

상기 목적을 달성하기 위한 본 발명은 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 700~900℃로 소성하여 산화마그네슘(산화마그네슘A)을 제조하는 단계;The present invention for achieving the above object is a step of producing magnesium oxide (magnesium oxide A) by baking magnesium hydroxide produced by reacting magnesium chloride and caustic soda at 700 ~ 900 ℃;

해수 또는 간수와 석회를 반응시켜 생성된 수산화마그네슘을 1000~1200℃로 소성하여 산화마그네슘(산화마그네슘B)을 제조하는 단계; 및Preparing magnesium oxide (magnesium oxide B) by calcining magnesium hydroxide produced by reacting seawater or brine with lime at 1000 to 1200 ° C; And

상기 산화마그네슘A: 35~45중량% 및 상기 산화마그네슘B: 55~65중량%를 혼합하는 단계;를 포함하는 방향성 전기강판용 소둔분리제의 제조방법에 관한 것이다.The magnesium oxide A: 35 to 45% by weight and the magnesium oxide B: 55 to 65% by weight of the mixture; relates to a method for producing an annealing separator for a grain-oriented electrical steel sheet comprising a.

이하, 본 발명을 상세하게 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

본 발명의 방향성 전기강판용 소둔분리제의 제조방법은 염화마그네슘으로부터 산화마그네슘을 제조하는 단계, 해수 또는 간수로부터 산화마그네슘을 제조하는 단계 및 상기 2종류의 산화마그네슘을 혼합하는 단계로 이루어진다.The method for producing an annealing separator for a grain-oriented electrical steel sheet according to the present invention comprises the steps of preparing magnesium oxide from magnesium chloride, preparing magnesium oxide from seawater or brine, and mixing the two kinds of magnesium oxide.

먼저, 본 발명에서는 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 700~900℃로 소성하여 산화마그네슘(산화마그네슘A)을 제조한다. 이때, 소성온도는 700~900℃로 제한하는 것이 바람직하다. 그 이유는 상기 소성온도가 700℃ 미만이면 산화마그네슘의 활성도가 너무 높아져 물과 쉽게 수화하여 최종 전기강판의 품질을 저해시키고, 900℃를 초과하면 결정화 및 소결성이 너무 높아져 혼합성이 저하되기 때문이다. 이와 같이 제조된 산화마그네슘은 고활성을 지녀 Si와의 반응이 용이하고, 입자의 분산성이 우수하여 균일한 피막을 형성할 수 있으므로 우수한 절연특성을 얻는데 기여하게 된다.First, in the present invention, magnesium hydroxide (magnesium oxide A) is prepared by calcining magnesium hydroxide produced by reacting magnesium chloride with caustic soda at 700 to 900 ° C. At this time, the firing temperature is preferably limited to 700 ~ 900 ℃. The reason is that when the firing temperature is less than 700 ° C, the activity of magnesium oxide is too high to easily hydrate with water, which hinders the quality of the final electrical steel sheet. . Magnesium oxide prepared as described above has high activity and is easy to react with Si, and excellent in dispersibility of particles to form a uniform film, thereby contributing to obtaining excellent insulating properties.

이후, 본 발명에서는 해수 또는 간수와 석회를 반응시켜 생성된 수산화마그네슘을 1000~1200℃로 소성하여 산화마그네슘(산화마그네슘B)을 제조한다. 이때, 소성온도는 1000~1200℃로 제한하는 것이 바람직하다. 그 이유는 상기 소성온도가 1000℃ 미만이면 활성도가 너무 높아지는 문제점이 있고, 1200℃를 초과하면 소성온도가 너무 높아 활성도가 너무 떨어짐으로써 부착성 및 피막특성이 저해되기 때문이다. 이와 같이 제조된 산화마그네슘은 강고한 피막을 형성할 수 있을 뿐만 아니라 수화를 방지할 수 있어 보다 안정적인 자성을 얻는데 기여하게 된다.Subsequently, in the present invention, magnesium hydroxide (magnesium oxide B) is prepared by calcining magnesium hydroxide produced by reacting seawater or brine with lime at 1000 to 1200 ° C. At this time, the firing temperature is preferably limited to 1000 ~ 1200 ℃. The reason for this is that if the firing temperature is less than 1000 ° C., the activity becomes too high. If the firing temperature is higher than 1200 ° C., the firing temperature is too high and the activity becomes too low, thereby degrading adhesion and coating properties. Magnesium oxide prepared in this way can not only form a firm film, but also prevent hydration, thereby contributing to obtaining more stable magnetism.

이후, 상기와 같이 제조된 산화마그네슘A와 산화마그네슘B를 적절하게 혼합하게 되며, 이때 산화마그네슘A는 35~45중량%, 산화마그네슘B는 55~65중량%의 양으로 혼합하는 것이 바람직하다. 그 이유는 상기 산화마그네슘A의 함량이 35중량% 미만이거나 산화마그네슘B의 함량이 65중량%를 초과하면 피막특성이 저해되고, 산화마그네슘A의 함량이 45중량%를 초과하거나 산화마그네슘B의 함량이 55중량% 미만이 면 자기특성이 저해되는 문제점이 있기 때문이다.Thereafter, the magnesium oxide A and magnesium oxide B prepared as described above may be appropriately mixed. At this time, the magnesium oxide A is preferably mixed in an amount of 35 to 45% by weight and the magnesium oxide B in an amount of 55 to 65% by weight. The reason is that when the content of magnesium oxide A is less than 35% by weight or the content of magnesium oxide B is more than 65% by weight, the coating properties are inhibited, and the content of magnesium oxide A is more than 45% by weight or the content of magnesium oxide B This is because if the amount is less than 55% by weight, there is a problem that the magnetic properties are inhibited.

본 발명에 이용되는 산화마그네슘의 활성도는 예를들면 40% 구연산 활성도로 100~350초인 것이 바람직하다. 상기 활성도가 100초 미만이면 전기강판의 피막 및 자기특성이 저하될 수 있으며, 350초를 초과하면 수화반응 과다 및 응집의 문제점이 있을 수 있다.The activity of magnesium oxide used in the present invention is preferably 100 to 350 seconds with 40% citric acid activity. If the activity is less than 100 seconds, the coating and magnetic properties of the electrical steel sheet may be reduced, and if it exceeds 350 seconds, there may be a problem of excessive hydration reaction and aggregation.

또한, 본 발명에 이용되는 산화마그네슘은 평균입경이 5㎛ 이하이고, 최대입경이 44㎛ 이하인 것이 바람직한데, 그 이유는 평균입경이 5㎛를 초과하거나 최대입경이 44㎛를 초과하면 Si와의 반응성이 저하되어 양호한 피막을 얻기 어려운 문제점이 있기 때문이다.In addition, the magnesium oxide used in the present invention preferably has an average particle diameter of 5 μm or less and a maximum particle size of 44 μm or less, because the reactivity with Si when the average particle size exceeds 5 μm or the maximum particle size exceeds 44 μm This is because there is a problem that it is lowered and a good film is hardly obtained.

본 발명에서는 상기와 같이 조성되는 전기강판 소둔분리제 100중량부에 대하여 1~3중량부의 TiO2를 추가로 첨가하는 것이 가능하다. 상기 TiO2는 전기강판과의 반응을 향상시키는데 유효한 성분으로, 그 첨가량이 상기 소둔분리제 100중량부에 대하여 1중량부 미만이면 첨가에 따른 상기 효과를 얻을 수 없고, 3중량부를 초과하면 소둔분리 효과를 저해시키는 문제점이 있다.In the present invention, it is possible to further add 1 to 3 parts by weight of TiO 2 based on 100 parts by weight of the electrical steel sheet annealing separator formed as described above. The TiO 2 is an effective component for improving the reaction with the electrical steel sheet, and when the amount is less than 1 part by weight based on 100 parts by weight of the annealing separator, the effect of the addition cannot be obtained. There is a problem that inhibits the effect.

또한, 본 발명에서는 상기와 같이 조성되는 전기강판 소둔분리제 100중량부 에 대하여 0.1~0.5중량부의 붕사(Na2B4O7)를 추가로 첨가하는 것이 가능하다. 상기 붕사는 반응촉진제로 작용하며, 그 첨가량이 소둔분리제 100중량부에 대하여 0.1중량부 미만이면 첨가에 따른 상기 효과를 얻을 수 없고, 0.5중량부를 초과하면 불순물이 증가되고 소결이 과다해지는 문제점이 있다.In addition, in the present invention, 0.1 to 0.5 parts by weight of borax (Na 2 B 4 O 7 ) may be further added to 100 parts by weight of the electrical steel sheet annealing separator prepared as described above. The borax acts as a reaction accelerator, and if the amount is less than 0.1 part by weight based on 100 parts by weight of the annealing separator, the effect of the addition cannot be obtained. If the amount exceeds 0.5 parts by weight, impurities increase and sintering is excessive. have.

이하, 실시예를 통하여 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

[실시예]EXAMPLE

해수와 석회를 반응시켜 생성된 수산화마그네슘을 1050℃, 1400℃ 및 450℃에서 소성하여 MgO①, MgO② 및 MgO④를 제조하였다. 또한, 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 800℃에서 소성하여 MgO③을 제조하였다.Magnesium hydroxide produced by reacting seawater with lime was calcined at 1050 ° C, 1400 ° C, and 450 ° C to prepare MgO①, MgO②, and MgO④. In addition, magnesium hydroxide produced by reacting magnesium chloride with caustic soda was calcined at 800 ° C. to prepare MgO③.

이후, 하기 표 1과 같이 조성된 전기강판 소둔분리제를 규소강판에 도포하고 건조한 다음, 1200℃에서 10시간동안 소둔을 실시하였다. 도포작업시 강판표면의 외관의 균일성은 육안으로 관찰하여 평가하였으며, 그 결과는 하기 표 1과 같다.Thereafter, the electrical steel sheet annealing separator prepared as shown in Table 1 was applied to the silicon steel sheet and dried, and then annealed at 1200 ° C. for 10 hours. The uniformity of the appearance of the steel sheet surface during the coating operation was observed by visual observation and evaluated, and the results are shown in Table 1 below.

또한, 시료를 채취하여 구연산 활성도, 평균입경, 최대입경을 측정하였으며, 그 결과는 하기 표 1과 같다. 또한 포스테라이트의 생성량을 측정하기 위하여 XRD 분석기를 이용하여 생성율을 측정하였으며, 그 결과는 하기 표 1과 같다.In addition, the sample was taken to measure the citric acid activity, average particle diameter, maximum particle size, the results are shown in Table 1 below. In addition, the production rate was measured using an XRD analyzer to measure the amount of forsterite produced, and the results are shown in Table 1 below.

상기 결과에 대하여 종합적으로 평가하여 현장적용 가능성 여부를 양호, 미비로 표시하였으며, 그 결과는 하기 표 1과 같다.By comprehensively evaluating the results, the possibility of field application was indicated as good or incomplete, and the results are shown in Table 1 below.

구분division 발명예1Inventive Example 1 발명예2Inventive Example 2 비교예1Comparative Example 1 비교예2Comparative Example 2 비교예3Comparative Example 3 MgO① (중량%)MgO① (wt%) 6060 5555 -- 6060 -- MgO② (중량%)MgO② (wt%) -- -- 6060 -- 6060 MgO③ (중량%)MgO③ (wt%) 4040 4545 -- -- 4040 MgO④ (중량%)MgO④ (wt%) -- -- 4040 4040 -- TiO2(외삽) (중량부)TiO 2 (extrapolated) (parts by weight) 22 22 22 22 22 Na2B4O7(외삽) (중량부)Na 2 B 4 O 7 (extrapolated) (parts by weight) 0.30.3 0.30.3 0.30.3 0.30.3 0.30.3 결 과    result 40%구연산 활성도(초)40% citric acid activity in seconds 210210 175175 380380 230230 320320 평균입경 (㎛)Average particle size (㎛) 33 2.52.5 55 44 1010 최대입경 (㎛)Particle size (㎛) 4444 4444 4444 4444 4444 피막외관Outer appearance 균일Uniformity 균일Uniformity 불균일Heterogeneity 불균일Heterogeneity 불균일Heterogeneity 포스테라이트 생성율(%)% Forsterite production 8888 9090 9292 8787 8686 현장적용 가능성Field applicability 양호Good 양호Good 미비Incomplete 미비Incomplete 미비Incomplete - MgO①: 해수와 석회를 반응시켜 생성된 수산화마그네슘을 1050℃에서 소성하여 제조 - MgO②: 해수와 석회를 반응시켜 생성된 수산화마그네슘을 1400℃에서 소성하여 제조 - MgO③: 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 800℃에서 소성하여 제조 - MgO④: 해수와 석회를 반응시켜 생성된 수산화마그네슘을 450℃에서 소성하여 제조-MgO①: Magnesium hydroxide produced by reacting seawater and lime at 1050 ℃-MgO②: Magnesium hydroxide produced by calcining seawater and lime at 1400 ℃-MgO③: Magnesium chloride and sodium hydroxide Magnesium hydroxide produced by firing at 800 ° C.-MgO ④: prepared by firing magnesium hydroxide produced by reacting seawater with lime at 450 ° C.

상기 표 1에 나타난 바와 같이, 본원발명에 따른 발명예1~2는 피막외관이 균일할 뿐만 아니라 포스테라이트 생성율이 높아 자기특성이 우수한 방향성 전기강판을 제조할 수 있었다.As shown in Table 1, Inventive Examples 1 and 2 according to the present invention were able to produce a grain-oriented electrical steel sheet having excellent magnetic properties as well as a uniform film appearance and high forsterite production rate.

그러나, 소성온도를 너무 낮게 하거나 너무 높게 한 비교예1~3의 경우 피막외관이 불균일하거나 포스테라이트 생성율이 낮아 자기특성이 저하되는 문제점이 발생하였다.However, in Comparative Examples 1 to 3, in which the firing temperature was too low or too high, the film appearance was uneven or the production rate of forsterite was low, resulting in a decrease in magnetic properties.

상술한 바와 같이, 본 발명에 따르면 균일한 피막특성 및 우수한 자기특성을 갖는 방향성 전기강판의 제조가 가능한 소둔분리제를 제공할 수 있다.As described above, according to the present invention, it is possible to provide an annealing separator capable of producing a grain-oriented electrical steel sheet having uniform coating properties and excellent magnetic properties.

Claims (5)

염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 700~900℃로 소성하여 산화마그네슘(산화마그네슘A)을 제조하는 단계;Preparing magnesium oxide (magnesium oxide A) by calcining magnesium hydroxide produced by reacting magnesium chloride with caustic soda at 700 to 900 ° C; 해수 또는 간수와 석회를 반응시켜 생성된 수산화마그네슘을 1000~1200℃로 소성하여 산화마그네슘(산화마그네슘B)을 제조하는 단계; 및Preparing magnesium oxide (magnesium oxide B) by calcining magnesium hydroxide produced by reacting seawater or brine with lime at 1000 to 1200 ° C; And 상기 산화마그네슘A: 35~45중량% 및 상기 산화마그네슘B: 55~65중량%를 혼합하는 단계;를 포함하는 방향성 전기강판용 소둔분리제의 제조방법.Mixing the magnesium oxide A: 35 to 45% by weight and the magnesium oxide B: 55 to 65% by weight; Method for producing an annealing separator for a grain-oriented electrical steel sheet comprising a. 제 1항에 있어서, 상기 산화마그네슘의 활성도는 40% 구연산 활성도로 100~350초인 것을 특징으로 하는 방향성 전기강판용 소둔분리제의 제조방법.The method of claim 1, wherein the magnesium oxide has a 40% citric acid activity of 100 to 350 seconds. 제 1항에 있어서, 상기 산화마그네슘은 평균입경이 5㎛ 이하이고, 최대입경이 44㎛ 이하인 것을 특징으로 하는 방향성 전기강판용 소둔분리제의 제조방법.The method of claim 1, wherein the magnesium oxide has an average particle diameter of 5 μm or less and a maximum particle size of 44 μm or less. 제 1항에 있어서, 상기 소둔분리제 100중량부에 대하여 1~3중량부의 TiO2를 추가로 첨가하는 것을 특징으로 하는 방향성 전기강판용 소둔분리제의 제조방법.The method of claim 1, wherein 1 to 3 parts by weight of TiO 2 is further added to 100 parts by weight of the annealing separator. 제 1항에 있어서, 상기 소둔분리제 100중량부에 대하여 0.1~0.5중량부의 붕 사를 추가로 첨가하는 것을 특징으로 하는 방향성 전기강판용 소둔분리제의 제조방법.The method of claim 1, wherein 0.1 to 0.5 parts by weight of borax is further added to 100 parts by weight of the annealing separator.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101052344B1 (en) * 2009-05-01 2011-07-27 한국기계연구원 Method for producing high purity magnesium oxide powder from magnesium chloride
KR101155606B1 (en) 2012-02-22 2012-06-13 삼화화학공업주식회사 Manufacturing process of magnesia for annealing separator of grain oriented electrical steel
KR20190042227A (en) 2017-10-16 2019-04-24 에스아이에스 주식회사 Manufacturing system for annealing separating agent
EP4206136A4 (en) * 2020-08-28 2024-02-28 Jfe Steel Corp Powder for annealing separator, method for producing same, and method for producing grain-oriented electrical steel sheet

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101052344B1 (en) * 2009-05-01 2011-07-27 한국기계연구원 Method for producing high purity magnesium oxide powder from magnesium chloride
KR101155606B1 (en) 2012-02-22 2012-06-13 삼화화학공업주식회사 Manufacturing process of magnesia for annealing separator of grain oriented electrical steel
KR20190042227A (en) 2017-10-16 2019-04-24 에스아이에스 주식회사 Manufacturing system for annealing separating agent
EP4206136A4 (en) * 2020-08-28 2024-02-28 Jfe Steel Corp Powder for annealing separator, method for producing same, and method for producing grain-oriented electrical steel sheet

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