KR910004116B1 - A testing method for the purity of slab - Google Patents

A testing method for the purity of slab Download PDF

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KR910004116B1
KR910004116B1 KR1019880017838A KR880017838A KR910004116B1 KR 910004116 B1 KR910004116 B1 KR 910004116B1 KR 1019880017838 A KR1019880017838 A KR 1019880017838A KR 880017838 A KR880017838 A KR 880017838A KR 910004116 B1 KR910004116 B1 KR 910004116B1
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specimen
inclusions
electrolytic
slab
cleanliness
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KR900010393A (en
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김동식
박학렬
정연대
안병관
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재단법인 산업과학기술연구소
박태준
포항제철 주식회사
정명식
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Abstract

A method for estimating a cleanliness of the cast slab comprises (a) grinding and cleaning a specimentaken from the cast slab, (b) electrolyzing the specimen for 20-30 minutes in an electrolytic soluton consisting of tetramethy ammonium chloride under the condition of 3-4 pH, 750-1300mA electric current, and (c) observing the specimen with the stereomicroscope and monitor.

Description

연속주조한 주편의 청정도 평가방법Cleanliness Evaluation Method of Continuous Casting

제 1 도는 본 발명의 전해처리를 수행하기 위한 전해장치개략도.1 is a schematic diagram of an electrolytic apparatus for carrying out the electrolytic treatment of the present invention.

제 2 도는 대형시편중 산화개재물의 형태를 나타내는 현미경사진.2 is a micrograph showing the shape of the oxidized inclusions in a large specimen.

제 3 도는 본 발명과 종래방법의 청정도평가시간을 비교한 그래프.3 is a graph comparing the cleanliness evaluation time of the present invention and the conventional method.

제 4 도는 시편중 개재물크기분포를 나타내는 분포도.4 is a distribution chart showing the distribution of inclusion sizes in a specimen.

본 발명은 연속주조한 주편의 청정도 평가방법, 보다 상세히는, 연속주조한 주편으로부터 채취된 대형시편중에 있는 비금속산화개재물의 청정도를 평가할 수 있는 연속주조한 주편의 청정도 평가방법에 관한 것이다.The present invention relates to a method for evaluating the cleanliness of continuously cast steel castings, and more particularly, to a method for evaluating the cleanliness of non-metal oxide inclusions in large specimens collected from continuously cast steel castings.

일반적으로 연속주조한 주편(Slab, bloom billet)중에 존재하는 비금속산화개재물(이하 개재물이라 칭함)들은 제강공정중 탈산생성물, 각종 슬래그내화물등의 형태로 있으면서 주조시 혼입된 것이다. 그러나 이러한 주편중 개재물들은 열간 및 냉간압연시 슬리버, 블랙라인들의 결합원인이 될뿐만 아니라 최종제품 가공시 프레시 결함등 각종 결함을 야기시킨다. 그러므로 주편중의 개재물의 형태, 크기, 갯수등의 청정도수준의 정확한 규명을 통해서 만이 그 기원을 분명하게 규명할 수 있고, 또한 이와 같은 개재물을 감소시킬 수 있는 효과적 대책수립이 가능하다. 뿐만 아니라 각종 저감대책에 대한 명확한 평가도 중요하다.In general, non-metal oxide inclusions (hereinafter referred to as inclusions) present in continuous cast slabs (slab, bloom billet) are mixed during casting, in the form of deoxidation products and various slag refractory materials during the steelmaking process. However, the inclusions in these castings are not only a cause of the combination of slivers and black lines in hot and cold rolling, but also cause various defects such as fresh defects in final product processing. Therefore, only the precise identification of the cleanliness level, such as the shape, size, and number of inclusions in the cast can clearly identify its origin, and it is possible to establish effective measures to reduce such inclusions. In addition, a clear evaluation of the various mitigation measures is important.

강중 개재물의 평가방법으로는 상분석(Image Analyzer)법과 일본특허공보 소 54-12240호등에 제시된 전해추출방법이 알려져 있다. 상기 상분석방법은 강시편을 연마한 후 광학현미경을 통하여 단위 면적중 개재물들이 차지하는 면적비율값을 얻거나, 또는 크기분포의 정보를 얻을 수 있지만, 시편의 크기(일반적으로, 10mm 가로×10mm 세로)가 크게 제한되어 연주주편과 같은 대형(macro) 시편(250mm 두께×100mm 가로)에 대한 평가는 곤란하며, 시편을 연마하여 2차원적으로 관찰하기 때문에 개재물의 실제크기, 형태의 관찰이 어려운 문제점이 있다.As a method for evaluating inclusions in steel, electrolytic extraction methods disclosed in Image Analyzer and Japanese Patent Publication No. 54-12240 are known. In the image analysis method, after polishing a steel specimen, an optical microscope can be used to obtain an area ratio value of inclusions in a unit area, or to obtain size distribution information. However, the size of the specimen (typically, 10 mm width × 10 mm length) ), It is difficult to evaluate macro specimens (250mm thickness × 100mm width) such as cast pieces, and it is difficult to observe the actual size and shape of inclusions because the specimens are polished and observed in two dimensions. There is this.

또한, 일본특허공보 소 54-12240호에 제시된 전해추출방법은 대형 시편의 크기에 대한 기재물의 실제크기, 형태는 알수있지만 시편을 용해하기 때문에 개재물의 위치파악이 어려우며 그 공정이 전해-잔사물의 술(Elutriation)-자석분리-수소환원-자석분리-염산처리등의 분리절차를 거쳐야하므로 적지않은 개재물의 손실을 쉽게 예상할 수 있고, 전해시간 및 모든 분리공정을 합하면 긴시간이 요구되므로 상기 청정도결과를 연주열간압연-냉간압연의 공정중 품질등급분류에 적용하기에는 불가능한 실정이다.In addition, the electrolytic extraction method presented in Japanese Patent Application Publication No. 54-12240 shows the actual size and shape of the substrate with respect to the size of the large specimen, but it is difficult to locate the inclusions because it dissolves the specimen. The separation process of elutriation, magnetic separation, hydrogen reduction, magnetic separation, hydrochloric acid treatment can be easily expected, and it is easy to anticipate the loss of many inclusions. It is impossible to apply the results to the in-process quality classification of hot rolling-cold rolling.

특히 잔사물의 수리분리공정은 스토크스(Stokes)법칙을 이용한 수리분석(Elutriation) 특징상 50㎛ 이상(일반적으로 대형 개재물이라함)의 개재물만 회수가 용이하며 50㎛ 이하의 미세 개재물에 대한 평가는 어려우며 강시편 전부를 전해에 의해 용해시키기 때문에 시편중 개재물의 정확한 위치 파악이 어려워 개재물의 혼입과정 규명 및 대책제시에 문제가 있다. 따라서, 본 발명은 연주주편 및 조괴(Ingot)재로부터 채취된 대형시편을 약전해한 후 스테레오현미경 및 현미경에 부착된 모니터를 이용하여 시편중 산화개재물을 3차원적으로 관찰하므로서 짧은 시간에보다 작은 크기의 개재물을 정확하게 평가할 수 있는 연속주조한 주편의 청정도를 평가하는 방법을 제공하고자 하는 것이다.In particular, the hydraulic separation process of residues is easy to recover only inclusions of 50 µm or more (generally called large inclusions) due to the characteristics of Elutriation using the Stokes law and evaluation of fine inclusions of 50 µm or less. It is difficult and difficult to pinpoint the inclusions in the specimen because it dissolves all of the steel specimens by electrolysis. Therefore, the present invention uses the monitor attached to the stereo microscope and microscope after weakly electrolyzing the large specimens collected from the playing cast and the ingot, and then the three-dimensional observation of the oxidized inclusions in the specimen is smaller than in a short time. It is intended to provide a method for evaluating the cleanliness of continuous cast steels that can accurately assess inclusions of size.

이하 본 발명을 상세히 설명한다. 본 발명은 연속주조한 주편으로부터 시편을 채취하여 연마 및 초음파 세척을 한 다음, 10-14wt%의 테트라메칠암모니움 클로라이드와 알콜용액으로 이루어진 전해용액에서 pH : 3.4- 및 전류 : 750mA-1300mA의 조건으로 20-30분동안 전해처리한 다음, 스테레오현미경과 모니터로 시편을 관찰하는 연속주조한 주편의 청정도 평가방법에 관한 것이다.Hereinafter, the present invention will be described in detail. According to the present invention, the specimens are taken from the continuously cast slab, polished, and ultrasonically cleaned, and then the pH is 3.4- and the current is 750 mA-1300 mA in an electrolytic solution consisting of 10-14 wt% tetramethylammonium chloride and an alcohol solution. This method relates to a method of evaluating the cleanliness of continuously cast steel castings after electrolysis for 20-30 minutes, and then observing the specimens with a stereo microscope and a monitor.

상기 전해처리방법을 제 1 도를 통하여 상세히 설명하면, 저해조(1)내에 양극은 강기편(2), 음극은 스테인레스판(3)을 각각 사용하고, 자동정전류방식으로 일정한 전류밀도를 유지하는 상기의 전해조건에 의해 시편으로부 개재물이 분리. 하부로 떨어지지않고, 시편상에 존재하는 개재물 경계면 주변의 Fe만을 일부 용해시키므로써 시편상에 개재물의 일부를 돌출시킨다.The electrolytic treatment method will be described in detail with reference to FIG. 1, in which the positive electrode is a steel piece 2 and the negative electrode is a stainless plate 3, respectively. The inclusions are separated from the specimen by the above electrolytic conditions. Instead of falling to the bottom, part of the inclusion is projected on the specimen by dissolving only Fe around the inclusion boundary on the specimen.

이와 같이 약전해된 시편을 건조시킨 후 스테레오현미경의 시편대에 올려놓고 일정한 배율로써 좌우상하로 이동시켜 가며 관찰하고 동시에 현미경에 부착된 모니터를 통해 개재물을 확인하고, 이들을 오버헤트프로젝터용 투명복사지상의 개재물크기기준표를 이용하여 실제크기를 파악하게 된다.After drying the weakly electrolyzed specimens, put them on the specimen stand of the stereo microscope and move them from side to side at a constant magnification. Observe the inclusions through the monitor attached to the microscope. The actual size will be determined by using the inclusion size standard table.

상기 전해용액은 유기용액인 테트라메칠암모니움 클로라이드(Tetramethyl Ammonium Chloride)+알콜용액으로 이루어지며, 이 용액을 이용하는 경우에는 양극표면에 산화층이 형성되어 전해가 일어나지 않는 부동태현상이 잘 일어나지 않게된다.The electrolyte solution consists of an organic solution, tetramethyl ammonium chloride (Tetramethyl Ammonium Chloride) + alcohol solution, when using this solution, an oxide layer is formed on the surface of the anode to prevent the passivation phenomenon does not occur easily.

상기 전해액의 조성, pH 및 전류는 시편 평면상에 분석하고자하는 개재물이 적절하게 노출되도록 제한되는 것으로서, 전해시에 시편중의 개재물이 분리되지 않고, 시편평면상의 불균일한 전해와 국부적인 전류밀도 차이등에 의한 요철현상, 및 개재물이 전해액에 의해 용해되지 않도록 해야한다.The composition, pH, and current of the electrolyte are limited so that the inclusions to be analyzed on the specimen plane are properly exposed, so that the inclusions in the specimen are not separated during electrolysis, and there is a difference in localized current density and uneven electrolysis on the specimen plane. Unevenness due to and the like, and inclusions should not be dissolved by the electrolyte solution.

이하, 실시예를 통하여 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.

[실시예 1]Example 1

저탄소 Al-Killed 강의 주편인 슬래브로부터 가로 100mm×두께 2500mm의 시편을 절단, 가공하여 연마한 다음, 초음파 세척후 제 1 도의 전해장치를 이용하여 하기표 1에 나타난 전해조건으로 전해처리를 행하였다.After cutting, processing and polishing a 100 mm × 2500 mm thick specimen from a slab, which is a slab of a low carbon Al-Killed steel, electrolytic treatment was performed under the electrolytic conditions shown in Table 1 using the electrolytic apparatus of FIG. 1 after ultrasonic cleaning.

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상기와 같이 전해처리된 시편을 현미경관찰하여 전해상태 및 개재물 돌출상태를 상기표 1에 나타내었다. 상기 표 1에 나타난 바와 같이 본 발명에 부합되는 전해조건으로 전해처리된 발명재 5-6 및 8-9는 비교재 1-4, 비교재 7, 및 비교재 10-12와는 달리, 차후의 스테레오 현미경과 모니터를 이용한 청정도평가공정에 적절한 전해시편임을 알 수 있다.The electrolytic state and the inclusion protrusion state are shown in Table 1 by microscopic observation of the electrolytically treated specimen as described above. Inventive materials 5-6 and 8-9 electrolytically treated under the electrolytic conditions according to the present invention as shown in Table 1, unlike Comparative material 1-4, Comparative material 7, and Comparative material 10-12, subsequent stereo It can be seen that the electrolytic specimen is suitable for the cleanliness evaluation process using a microscope and a monitor.

[실시예 2]Example 2

저탄소 Al-Killed 강주편인 슬래브로부터 가로 100mm×세로 250mm×두께 5mm의 크기로 시편을 채취하여 표면가공한 후 초음파세척하여 10% 테트라메칠 암모니움 클로라이드+알콜로 이루어진 전해액에서 800mA의 전류, 800mV의 전압 및 pH 4의 전해조건에서 약 30분간 전해하였다.The specimen was taken from the slab, a low carbon Al-Killed steel slab, 100mm wide x 250mm long and 5mm thick, and surface treated, and then ultrasonically cleaned to obtain 800mA current and 800mV current in an electrolyte consisting of 10% tetramethyl ammonium chloride + alcohol. Electrolysis was carried out for about 30 minutes at the voltage and electrolysis conditions of pH 4.

전해처리가 완료된 시편을 알콜로 세척하고 건조후 현미경시편대에 올려놓고, 좌, 우, 상, 하로 이동하여 가면서 배율×50배로 하여 1차적으로 현미경대물렌즈 및 대안렌즈에 의해 관찰하면서 동시에 모니터에 나타난 산화개재물을 확인하여 제 2 도에 나타내었으며 제 2 도와 같이 대형시편상에 나타난 산화개재물의 분포상태를 종래의 방법과 함께 제 4 도에 나타내었다. 제 4 도에 나타난 바와 같이, 본 발명에 의한 평가방법은 종래방법에 비하여 아주 미세한 크기의 산화개재물도 평가할 수 있음을 알 수 있다. 또한, 본 발명에 의한 평가방법에 소요되는 시간을 종래방법과 비교하여 제 3 도에 나타내었는데, 이로부터 알 수 있는 바와 같이, 본 발명이 종래방법보다 평가에 소요되는 시간이 적게 걸림을 알 수 있다.After the electrolytic treatment is completed, the specimen is washed with alcohol, dried and placed on the microscope specimen stage. The magnification is 50x while moving left, right, up, and down, and is primarily observed by the microscope objective lens and the alternative lens. The oxidation inclusions shown were identified in FIG. 2 and the distribution state of the oxidation inclusions shown on the large specimens as shown in FIG. 2 is shown in FIG. 4 along with the conventional method. As shown in Figure 4, it can be seen that the evaluation method according to the present invention can also evaluate the oxidation inclusions of a very fine size compared to the conventional method. In addition, the time required for the evaluation method according to the present invention is shown in FIG. 3 in comparison with the conventional method. As can be seen from this, it can be seen that the present invention takes less time for evaluation than the conventional method. have.

상술한 바와 같이, 본 발명은 적절한 조건으로 전해처리하고 스테레오 현미경과 모니터로 관찰하여 청정도를 평가하므로서 청정도 평가시간이 현저히 감소될뿐만 아니라 개재물의 위치형상 및 미세한 산화개재물까지도 관찰할 수 있는 효과가 있는 것이다.As described above, the present invention not only significantly reduces the cleanliness evaluation time by electrolyzing under appropriate conditions and observing with a stereo microscope and monitor, but also has the effect of observing the positional shape of the inclusions and even fine oxidation inclusions. It is.

Claims (1)

연속주조한 주편으로부터 시편을 채취하여 연마 및 세척한 다음, 10-14wt%의 테트라메칠암모늄클로라이드와 알콜 용액으로 이루어진 전해용액에서 pH : 3-4 및 전류 750mA-1300mA의 조건으로 20-30분동안 전해처리한 다음, 스테레오 현미경과 모니터로 시편을 관찰하는 것을 특징으로 하는 연속주조한 주편의 청정도 평가방법.The specimens were taken from the continuously cast slabs, polished and washed, and then in an electrolyte solution consisting of 10-14 wt% tetramethylammonium chloride and an alcohol solution for 20-30 minutes under the conditions of pH 3-4 and current 750 mA-1300 mA. Cleanliness evaluation method of the continuously cast cast, characterized in that after the electrolytic treatment, the specimen is observed with a stereo microscope and a monitor.
KR1019880017838A 1988-12-29 1988-12-29 A testing method for the purity of slab KR910004116B1 (en)

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