KR20080040340A - Method for manufacturing silicon steel sheets with a high silicon content by the decomposition of sio2 and the subsequent silicon diffusion during an annealing under hydrogen atmosphere - Google Patents
Method for manufacturing silicon steel sheets with a high silicon content by the decomposition of sio2 and the subsequent silicon diffusion during an annealing under hydrogen atmosphere Download PDFInfo
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Abstract
Description
도 1은 두께 0.1 mm의 전해철 강판에서 실리카 분말 도포제의 침투 확산법에 의해 주입되는 규소의 양과 고온(1200℃)의 수소(2 liter/min)분위기에서 열처리하는 시간과의 관계를 나타낸 그래프이다. 대략 10시간당 1 wt%가 주입됨을 알 수 있다.1 is a graph showing the relationship between the amount of silicon injected by the penetration diffusion method of the silica powder coating agent in a 0.1 mm thick electrolytic iron sheet and the time of heat treatment in a hydrogen (2 liter / min) atmosphere at a high temperature (1200 ° C.). It can be seen that approximately 1 wt% is injected per 10 hours.
도 2는 두께 0.1 mm의 규소강판(규소함량 3%)에서 실리카 분말 도포제의 침투 확산법에 의해 주입되는 규소의 양과 고온(1200℃)의 수소(2 liter/min)분위기에서 열처리하는 시간과의 관계를 나타낸 그래프이다. 전해철의 경우와 유사하게 대략 10시간당 1 wt%가 주입됨을 알 수 있다.2 is a relation between the amount of silicon injected by the penetration diffusion method of the silica powder coating agent on a 0.1 mm thick silicon steel sheet (
본 발명은 각종 전기기계의 철심재료로 사용되는 전기강판의 규소함량을 높여 철손을 획기적으로 줄일 수 있는 고규소 강판 제조방법에 관한 것으로서, 통상 의 실리카 분말을 전해철 또는 규소를 일정량 함유하고 있는 규소강판에 슬러리 형태로 도포한 후 건조하여 고온의 수소분위기에서 규소를 침투 확산시킴으로써 상용주파수에서 고주파영역에 이르기까지 철손특성이 우수한 이산화규소의 분해 및 침투 확산에 의한 고규소 강판 제조방법에 관한 것이다.The present invention relates to a method for producing a high silicon steel sheet that can significantly reduce iron loss by increasing the silicon content of the electrical steel sheet used as iron core materials of various electric machines, and a silicon steel sheet containing a predetermined amount of electrolytic iron or silicon in a conventional silica powder The present invention relates to a method for manufacturing a high silicon steel sheet by dissolving and infiltrating diffusion of silicon dioxide having excellent iron loss characteristics from a commercial frequency to a high frequency region by applying silicon in a slurry form and drying to penetrate and diffuse silicon in a high temperature hydrogen atmosphere.
규소강판에서 규소함량이 증가할수록 와전류 손실이 감소하여 철손특성이 개선되며, 규소함량 6.5%에서 소음과 관계된 자왜의 감소 및 최대 투자율의 증가가 최고치를 나타냄으로써 6.5% 규소강판이 우수한 자기적 특성을 갖는 것은 이미 널리 알려진 사실이다. 이러한 사실에도 불구하고 극히 제한적으로 고규소 전기강판이 사용되는 이유는 규소함량이 3%를 넘게 되면 취성이 증가하여 냉간압연이 곤란하므로 통상적인 냉간압연법에 의한 고규소 전기강판 제조는 현실적으로 불가능한 상황이기 때문이다.As silicon content increases in silicon steel, eddy current loss decreases to improve iron loss characteristics.In 6.5% silicon content, 6.5% silicon steel exhibits excellent magnetic properties as the maximum magnetic permeability decrease and noise increase Having is a well known fact. In spite of this fact, the reason why extremely high quality silicon steel sheet is used is that when the silicon content exceeds 3%, the brittleness increases and cold rolling is difficult. Therefore, the production of high silicon electrical steel sheet by ordinary cold rolling method is practically impossible. Because it is.
현재 고규소 전기강판으로 사용되는 것은 SiCl4 가스를 이용한 화학증착법을 적용시킨 무방향성 6.5% 규소강판이 있다. 그러나 이 기술은 상업화 적용에 어려움이 많아 최종 제품의 가격이 매우 고가여서 3% 규소강판에 비해 거의 사용되지 않고 있다. 그 외에도 여러 가지 규소주입에 관한 기술이 특허로 소개되었으나 아직 실용화제품에 적용되는 기술은 없는 실정이다.Currently, high silicon electrical steel sheet is a non-oriented 6.5% silicon steel sheet using a chemical vapor deposition method using SiCl 4 gas. However, this technology is difficult to apply to commercialization, and the final product is very expensive, so it is rarely used compared to 3% silicon steel sheet. In addition, various silicon injection technologies have been introduced as patents, but there is no technology applied to commercialized products.
따라서 본 발명은 종래기술의 한계를 극복하기 위해 창안된 것으로서, 모 재료의 결정학적 방향성과 규소함유량에 관계없이 통상의 실리카 분말을 물과 조합 하여 슬러리 형태로 모 재료인 강판표면에 도포한 후, 고온의 수소분위기에서 분해된 규소를 침투 확산시킴으로써 용이하게 철손특성이 우수한 고규소 강판을 제조할 수 있는 방법을 제공하는데 그 목적이 있는 것이다.Therefore, the present invention was devised to overcome the limitations of the prior art, and after applying ordinary silica powder in combination with water to the surface of the steel sheet as the mother material, regardless of the crystallographic orientation and silicon content of the parent material, It is an object of the present invention to provide a method for easily producing a high silicon steel sheet having excellent iron loss characteristics by penetrating and diffusing silicon decomposed in a high temperature hydrogen atmosphere.
상기의 목적을 달성하기 위해 본 발명은 먼저 통상의 실리카 분말을 물과 조합하여 슬러리 형태의 실리카 분말도포제를 조제하는 바, 사용되는 실리카 분말의 순도와 입도는 모 재료와의 반응성에 따라 다양하게 준비될 수 있으며 일반적으로 순도에 따라 규소 주입효율이 달라지는데 입도가 작을수록 규소 주입 후 강판 표면의 평탄도가 좋다.In order to achieve the above object, the present invention first prepares a silica powder coating agent in the form of a slurry by combining ordinary silica powder with water, and the purity and particle size of the silica powder to be used vary depending on the reactivity with the parent material. In general, the silicon injection efficiency depends on the purity, the smaller the particle size, the better the flatness of the surface of the steel sheet after silicon injection.
상기의 실리카 분말도포제를 최종 목표로 하는 두께의 전해철 또는 규소를 일정량 함유하고 있는 규소강판 표면에 도포한 후 건조하여 권취한다. 코일형태로 권취한 강판을 수소분위기의 고온에서 장시간 열처리하게 되면 실리카 분말도포제는 수소와 반응하여 가스상태의 규소로 분해되고 결국 강판표면에 침투하여 내부로 확산하게 된다. 주입되는 규소의 양은 열처리 시 공급되는 수소의 양, 열처리 온도, 열처리 시간에 의해서 결정되므로 본 발명은 규소를 함유하지 않은 전해철 강판, 방향성 규소강판, 무방향성 규소강판 등에 모두 적용할 수 있는 장점을 가지고 있다.The silica powder coating agent is applied to the surface of a silicon steel sheet containing a predetermined amount of electrolytic iron or silicon having a thickness as a final target, and then dried and wound up. When the steel sheet wound in a coil form is heat-treated at a high temperature in a hydrogen atmosphere for a long time, the silica powder coating agent reacts with hydrogen to decompose into gaseous silicon, and eventually penetrates the surface of the steel sheet and diffuses therein. Since the amount of silicon to be injected is determined by the amount of hydrogen supplied during the heat treatment, the heat treatment temperature, and the heat treatment time, the present invention has the advantage that it can be applied to all of the silicon-free electrolytic iron sheet, the oriented silicon steel sheet, and the non-oriented silicon steel sheet. have.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
전기강판 제조공정은 최종 제품두께로 냉간압연을 실시한 후 적절한 마무리 소둔공정을 통해 전기강판의 자기적 특성을 확보한다. 이때 전기강판의 규소함유량 은 3.5%정도를 유지하게 되는데 이것은 규소의 함유량이 3.5%를 초과하게 되면 냉간압연이 곤란하기 때문이다.The electrical steel sheet manufacturing process is cold rolled to the final product thickness, and then secures the magnetic properties of the electrical steel sheet through an appropriate finishing annealing process. At this time, the silicon content of the electrical steel sheet is maintained at about 3.5% because the cold rolling is difficult when the silicon content exceeds 3.5%.
이에 본 발명자는 제품의 두께를 줄여 와전류손실을 줄이려는 연구를 진행하던 중, 주성분이 SiO2인 고순도 석영 튜브 내에서 규소강판을 고온의 건수소분위기에서 장시간 열처리 하면 규소강판 내의 규소함유량이 증가한다는 사실을 접하게 되었으며, 그 결과로 실리카 분말을 물과 조합한 슬러리 형태의 실리카 분말도포제를 규소강판 표면에 도포한 후 고온의 수소분위기, 예를 들면 1000 ~ 1400℃에서 장시간 열처리하여 규소함유량을 높일 수 있음을 실험적으로 확인하고 본 발명을 제안하게 되었다.Therefore, the present inventors have been researching to reduce the eddy current loss by reducing the thickness of the product, and the silicon content in the silicon steel sheet increases when the silicon steel sheet is heat-treated in a high temperature dry hydrogen atmosphere for a long time in a high purity quartz tube whose main component is SiO 2 . As a result, the silica powder coating agent in the form of slurry in which silica powder was combined with water was applied to the surface of the silicon steel sheet, and then heat-treated in a high temperature hydrogen atmosphere, for example, 1000 to 1400 ° C., to increase the silicon content. Experimentally confirmed that the present invention was proposed.
본 발명의 장점은 모 재료의 자기적 특성, 두께, 규소 함유량에 구애받지 않고 적용할 수 있다는 것이다. 특히 현재 상용화되고 있는 전기강판의 두께가 0.23 mm로 제한되고 있는 상황에서 0.1 mm 이하의 두께를 갖는 강판에도 본 발명에서 제안된 기술을 적용할 수 있으므로 고규소 특성으로 인한 철손개선효과 이외에도 두께감소에 의한 철손개선효과를 추가적으로 실현할 수 있는 장점이 있는 것이다.An advantage of the present invention is that it can be applied regardless of the magnetic properties, thickness and silicon content of the parent material. In particular, the present invention can be applied to the steel sheet having a thickness of 0.1 mm or less in the situation that the current commercial steel sheet thickness is limited to 0.23 mm, in addition to the iron loss improvement effect due to high silicon characteristics, There is an advantage that can additionally realize the iron loss improvement effect.
이하, 실시 예를 통하여 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.
(실시예 1)(Example 1)
두께 2.5 mm의 전해철 열연강판을 산세과정을 거쳐 중간소둔을 포함한 3회의 냉간압연을 통해 최종 두께 0.1 mm의 전해철 냉연강판을 만들었다. 이 냉연강판 표면에 순도 99.9%, 평균입도 20㎛의 실리카 분말을 물과 1:8(실리카 중량과 물의 중 량비)의 비율로 혼합하여 슬러리 형태의 실리카 분말도포제를 도포한 후 건조하였다.The hot rolled electrolytic iron sheet having a thickness of 2.5 mm was pickled and subjected to three cold rolling including intermediate annealing to produce an electrolytic iron cold rolled steel having a final thickness of 0.1 mm. Silica powder having a purity of 99.9% and an average particle size of 20 µm was mixed on the surface of the cold rolled steel sheet in a ratio of 1: 8 (weight ratio of silica weight and water) to apply a slurry-type silica powder coating agent and dried.
이어, 상기의 실리카 분말도포제가 도포된 전해철 냉연강판을 99.9999%의 고순도 건수소를 분당 2 liter를 흘리는 분위기에서 1200℃까지 승온하고 1200℃를 유지한 상태에서 도 1에 나타낸 바와 같이 열처리 시간을 달리하여 시편에 주입된 규소의 양을 중량%로 분석하였다.Subsequently, the electrolytic iron cold rolled steel sheet coated with the silica powder coating agent was heated to 1200 ° C in an atmosphere of flowing 99.9999% of high purity dry hydrogen at 2 liters per minute and maintained at 1200 ° C. The amount of silicon injected into the specimen was analyzed by weight percent.
첨부 도면 중 도 1은 두께 0.1 mm의 전해철 강판에서 실리카 분말 도포제의 침투 확산법에 의해 주입되는 규소의 양과 고온(1200℃)의 수소(2 liter/min)분위기에서 열처리하는 시간과의 관계를 나타낸 그래프이다. In the accompanying drawings, FIG. 1 is a graph showing the relationship between the amount of silicon injected by the penetration diffusion method of a silica powder coating agent in a 0.1 mm thick electrolytic iron sheet and the time of heat treatment in a hydrogen (2 liter / min) atmosphere at a high temperature (1200 ° C.). to be.
이상의 결과로부터 열처리 시간이 길어질수록 시간당 규소주입량이 다소 증가하긴 했으나 대략적으로 10시간당 1 중량% 정도의 규소가 주입됨을 확인하였다.From the above results, although the amount of silicon injection per hour increased slightly as the heat treatment time increased, it was confirmed that about 1 wt% of silicon was injected per 10 hours.
(실시예 2)(Example 2)
진공 유도용해로를 이용하여 3%의 규소가 함유된 잉곳을 제조한 후, 열간압연을 실시하여 두께 2.5 mm의 3% 규소 열연강판을 제조하였다. 두께 2.5 mm의 3% 규소 열연강판을 산세과정을 거쳐 중간소둔을 포함한 3회의 냉간압연을 통해 최종 두께 0.1 mm의 3% 규소 냉연강판을 만들었다. 이 냉연강판 표면에 순도 99.9%, 평균입도 20㎛의 실리카 분말을 물과 1:8(실리카 중량과 물의 중량비)의 비율로 혼합하여 슬러리 형태의 실리카 분말도포제를 도포한 후 건조하였다.After the ingot containing 3% silicon was manufactured using a vacuum induction furnace, hot rolling was performed to prepare a 3% silicon hot rolled steel sheet having a thickness of 2.5 mm. A 3% silicon hot rolled steel sheet with a thickness of 2.5 mm was pickled and subjected to cold rolling three times including intermediate annealing to make a 3% silicon cold rolled steel sheet with a final thickness of 0.1 mm. Silica powder having a purity of 99.9% and an average particle size of 20 µm was mixed on the surface of the cold rolled steel sheet in a ratio of 1: 8 (weight ratio of silica weight and water) to water to apply a slurry silica powder coating agent and then dried.
이어, 상기의 실리카 분말도포제가 도포된 3% 규소 냉연강판을 99.9999% 이상의 고순도 건수소를 분당 2 liter를 흘리는 분위기에서 1200℃까지 승온하고 1200℃를 유지한 상태에서 도 2에 나타낸 바와 같이 열처리 시간을 달리하여 시편에 주입된 규소의 양을 중량%로 분석하였다.Then, the 3% silicon cold rolled steel sheet coated with the silica powder coating agent was heated to 1200 ° C in an atmosphere of flowing 2 liters per minute of high purity dry hydrogen of 99.9999% or more, and the heat treatment time as shown in FIG. 2 while maintaining 1200 ° C. By varying the amount of silicon injected into the specimen was analyzed by weight%.
도 2는 두께 0.1 mm의 규소강판(규소함량 3%)에서 실리카 분말 도포제의 침투 확산법에 의해 주입되는 규소의 양과 고온(1200℃)의 수소(2 liter/min)분위기에서 열처리하는 시간과의 관계를 나타낸 그래프이다. 2 is a relation between the amount of silicon injected by the penetration diffusion method of the silica powder coating agent on a 0.1 mm thick silicon steel sheet (
이상의 결과로부터 실시예 1과 유사한 규소주입 효과를 얻을 수 있었으며 규소주입량도 대략적으로 10시간당 1 중량% 정도로 실시예 1과 유사하였다.The silicon injection effect similar to Example 1 was obtained from the above result, and the silicon injection amount was similar to Example 1 as about 1 weight% per 10 hours.
상술한 바와 같이, 본 발명은 통상의 실리카 분말을 이용해 규소를 전혀 함유하지 않은 전해철 또는 3.5% 정도까지 규소를 함유하고 있는 규소강판에 용이하게 규소를 주입할 수 있는 방법을 제공함으로써 자기적 특성이 우수한 것으로 알려진 고규소 강판을 제조할 수 있는 효과가 있다.As described above, the present invention provides a method of easily injecting silicon into an electrolytic iron containing no silicon or a silicon steel sheet containing up to about 3.5% silicon using a conventional silica powder, thereby improving magnetic properties. There is an effect that can produce a high silicon steel sheet known to be excellent.
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