KR960008154B1 - Method for manufacturing a electro-zinc plating steel sheets with an excellent surface brightness - Google Patents

Method for manufacturing a electro-zinc plating steel sheets with an excellent surface brightness Download PDF

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KR960008154B1
KR960008154B1 KR1019930030259A KR930030259A KR960008154B1 KR 960008154 B1 KR960008154 B1 KR 960008154B1 KR 1019930030259 A KR1019930030259 A KR 1019930030259A KR 930030259 A KR930030259 A KR 930030259A KR 960008154 B1 KR960008154 B1 KR 960008154B1
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chloride
plating
zinc
electro
plating bath
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KR1019930030259A
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KR950018678A (en
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김명수
안덕수
김영봉
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김종진
포항종합제철주식회사
신창식
재단법인산업과학기술연구소
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

This process manufactured the steel sheet of good surface brightness or high reflection of light by continuous electro-plating without adding brightener and controlling of various ion concentrations in plating solution. The good surface brightness is formed obtained by decreasing the crystal size of zinc, and increasing the degree of preferred gradient of zinc in this process. The conditions of plating are that: (a) the plating bath is of chloride system, (b) the pH of plating solution is 3 to 7, (c) the temperature of plating bath is 40 to 60deg.C, (d) the concentration of zinc chloride is 100 to 150g/L, and/or (e) the added conductive aiders are potassium chloride and ammonium chloride, and/or (f) the concentration of aiders is up to 100g/L, and (g) the degree of preferred gradient in the zinc base plane of the highest atomic density is over 6.

Description

표면강택성이 우수한 전기아연도금강판의 제조방법Manufacturing method of electrogalvanized steel sheet with excellent surface toughness

본 발명은 표면광택성이 우수한 전기아연도금강판의 제조방법에 관한 것으로서, 보다 상세하게는 염화물계 도금욕을 사용한 연속 전기아연도금시 광택제를 첨가하지 않고 도금용액중의 각종 이온 농도를 조절함으로서 전착아연결정의 크기를 감소시켜 도금후 표면광택성이 우수한 전기아연도금강판의 제조방법에 관한 것이다.The present invention relates to a method for producing an electrogalvanized steel sheet having excellent surface glossiness, and more particularly, to electrodeposition by controlling various ion concentrations in a plating solution without adding a polishing agent in continuous electroplating using a chloride plating bath. The present invention relates to a method for producing an electrogalvanized steel sheet having excellent surface glossiness after plating by reducing the size of zinc crystals.

일반적으로 전기아연도금강판을 생산하기 위한 도금욕은 주로 황산계와 염화물계 도금욕을 사용하는데, 염화물계 도금욕은 황산계 도금욕에 비해 욕저항이 작아 전류효율이 증가하여 고전류밀도 조업에 유리한 장점이 있는 반면, 전착결정이 황산계 도금욕에 비해 비교적 조대하고 불균일하여 광택도가 떨어지는 단점이 있다.In general, the plating bath for producing electro-galvanized steel sheet mainly uses sulfuric acid and chloride plating bath. Chloride plating bath is advantageous for high current density operation because the bath resistance is smaller than the sulfuric acid plating bath, so the current efficiency is increased. On the other hand, the electrodeposition crystals are relatively coarse and uneven compared to the sulfuric acid-based plating baths, and thus have a disadvantage of poor glossiness.

또한, 연속 아연도금설비에 있어서 염화물계 도금용액중에 염화아연의 농도는 180-250g/ℓ, 전도보조제인 염화칼륨 혹은 염화암모늄의 농도는 250-350g/ℓ 정도로 하여 도금하게 되는데, 상기와 같은 농도에서는 강판표면에 아연결정의 성장속도가 크기 때문에 결정립이 조대하며 또한 무질서한 형태로 성장하므로서 표면광택성이 떨어지는 문제점이 있다.In the continuous zinc plating equipment, the zinc chloride concentration in the chloride plating solution is 180-250 g / l, and the concentration of potassium chloride or ammonium chloride, a conduction aid, is about 250-350 g / l. Since the growth rate of zinc crystals on the surface of the steel sheet is large, there is a problem that the surface glossiness is inferior as the grains grow coarse and grow in a disordered form.

염화물계 도금욕을 사용하는 경우 전기아연도금강판의 광택성을 높이기 위하여, 종래에는 유기 또는 무기광택제를 도금액에 첨가하는 방법을 사용하였다. 이 방법에 의하면, 광택제를 도금액에 첨가함으로써, 이 광택제가 도금층의 조도를 감소시키게 되고, 따라서 강판표면에서 빛이 산란되는 비율을 감소시키므로서 표면광택성을 확보하는 것이었다. 그러나, 광택제를 첨가하는 경우 도금효율의감소, 표면색상의 변색 등의 문제뿐만 아니라, 첨가제가 섞임으로 인하여 도금층의 응력증가에 의한 성형시 균열이 발생되는 심각한 문제점이 있었다.In the case of using a chloride plating bath, in order to increase the glossiness of an electrogalvanized steel sheet, a method of adding an organic or inorganic varnish to a plating solution has been conventionally used. According to this method, by adding a polishing agent to the plating liquid, the polishing agent reduces the roughness of the plating layer, thereby securing the surface glossiness by reducing the rate at which light scatters on the surface of the steel sheet. However, when the brightening agent is added, not only problems such as reduction of plating efficiency and discoloration of the surface color, but also a serious problem of cracking during molding due to an increase in stress of the plating layer due to mixing of additives.

상기한 광택제를 첨가하지 않고 도금조건을 조절하여 광택성을 높이는 종래의 방법으로, 일본 공개특허공보(평) 4-9495호에 게제된 제안을 들 수 있는데, 이 방법은 통전량(전류×시간)을 7000c/dm2이상의 고전류로서 강판을 전해연마하여 황산계 도금욕에서 도금하는 방법이다. 이 방법의 경우에는 큰 통전량으로 인하여 전력사용비용의 상승은 물론 철 용해량 증가로 인한 제품의 단중(unit load) 감소, 전해용액의 오염속도 증가에 의한 잦은 전해액 교환의 필요성등으로 고속으로 연속도금하는 설비에 직용하기가 매우 어려운 것이다.As a conventional method of improving the glossiness by adjusting the plating conditions without adding the above-described polishing agent, there is a proposal published in Japanese Patent Application Laid-Open No. 4-9495. ) Is plated in a sulfuric acid plating bath by electropolishing steel sheet with a high current of 7000c / dm 2 or more. In the case of this method, due to the large current, the power consumption cost is increased, as well as the unit load of the product due to the increased iron dissolution and the need for frequent exchange of electrolyte due to the increase of the contamination rate of the electrolyte. It is very difficult to apply directly to the plating equipment.

따라서, 본 발명은 상기한 종래의 문제점을 해결하고자 제안된 것으로서, 연속도금라인에서 염화물계 도금욕에 광택제를 첨가하지 않고, 도금용액중의 각 이온들의 농도를 조절함으로서, 아연결정을 미세화시키고 표면에 아연기저면의 우선배향성을 증가시켜 광택성을 높여 표면광택성이 우수한 전기아연도금강판의 제조방법을 제공하고자 하는데, 그 목적이 있다.Accordingly, the present invention has been proposed to solve the above-described problems, and by adjusting the concentration of each ion in the plating solution without adding a polishing agent to the chloride-based plating bath in the continuous plating line, to refine the zinc crystals and the surface The purpose of the present invention is to provide a method for producing an electro-galvanized steel sheet having excellent surface glossiness by increasing the preferential orientation of the zinc base surface.

이하, 본 발명에 대하여 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated.

본 발명은, 염화물계 도금욕을 사용하고, 통상의 도금조건인 pH를 3-7, 도금욕의 온도를 40-60℃로 하여 연속 전기아연도금하는 전기아연도금강판의 제조방법에 있어서, 상기 염화물계 도금욕중의 염화아연 농도가 100-150g/ℓ이 되도록 조성하여 연속 전기아연도금하는 것을 특징으로 하는 표면광택성이 우수한 전기아연도금강판의 제조방법에 관한 것이다.The present invention relates to a method for producing an electro-zinc plated steel sheet which is subjected to continuous electro-galvanization using a chloride plating bath and having a pH of 3-7 and a temperature of 40-60 ° C., which are ordinary plating conditions. The present invention relates to a method for producing an electro-zinc plated steel sheet having excellent surface gloss, characterized in that the zinc chloride concentration in the chloride-based plating bath is 100-150 g / l and continuously electro-galvanized.

또한, 본 발명은 상기한 본 발명에 따른 도금욕에 전도보조제로 염화칼륨 및 염화암모늄을 단독 또는 혼합첨가하여 상기 전도보조제의 농도가 100g/ℓ 이하가 되도록 조성하여 연속 전기아연도금하는 것을 특징으로 하는 표면광택성이 우수한 전기아연도금강판의 제조방법에 관한 것이다.In addition, the present invention is characterized in that the plating bath according to the present invention is added to the potassium chloride and ammonium chloride as a conduction aid alone or mixed, so that the concentration of the conduction adjuvant is 100g / L or less to continuously electro-galvanized The present invention relates to a method for producing an electrogalvanized steel sheet having excellent surface glossiness.

이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

일반적으로 아연도금강판의 광택성은 아연결정의 크기와 결정의 우선배향도에 따라 다르다. 즉, 아연도금강판의 결정이 작을수록, 원자밀도가 가장 높은 아연기저면의 우선배향도가 클수륵 표면에서 빛의 반사도가 증가하기 때문에 광택성이 증가하는 것이다.In general, the glossiness of galvanized steel sheet depends on the size of zinc crystals and the preferred orientation of the crystals. In other words, the smaller the crystal of the galvanized steel sheet, the higher the degree of preferential orientation of the zinc base surface having the highest atomic density.

도금층 우선배향도는 X선(Cu-Kα) 회절분석기를 이용하여 회절강도를 측정한 후, 아래 식을 사용하여 나타내는데 이 우선 배향도는 도금층 표면에 평행한 면의 분포 정도를 의미하며, 아연기저면의 우선배향도가 6 이상이 되어야 본 발명에서 요구하는 광택도를 확보할 수 있다.The preferred orientation of the plated layer is measured using the X-ray (Cu-Kα) diffractometer and the following equation is used. The preferred orientation represents the degree of distribution of the plane parallel to the surface of the plated layer. Orientation degree should be 6 or more to ensure the glossiness required by the present invention.

여기에서,From here,

I(hkl): 실험시편의 (hkl)면에 대한 회절강도I (hkl) : diffraction intensity on the (hkl) plane of the test specimen

Io(hkl): 표준시료의 (hkl)면에 대한 회절강도I o (hkl) : diffraction intensity on (hkl) plane of standard sample

n : 조사된 면들의 갯수, 본 발명에서는 10개n: number of irradiated faces, in the present invention 10

본 발명은 염화물계 도금욕중에 염화아연의 농도를 100-150g/ℓ로 조성하거나, 또는 상기의 염화아연 농도에 전도보조제인 염화칼륨 및 염화암모늄을 단독 혹은 혼합하여 첨가하여 전도보조제의 농도를 100g/ℓ 이하로 해줌으로써, 아연이온의 석출과전압을 증가시켜서, 이로 인해 아연결정의 성장속도가 감소되어, 결과적으로 아연결정의 크기를 감소시키고, 또한 표면에 평행한 아연기저면의 우선배향성을 6 이상으로 증가시켜서 광택도가 증가시키는 것을 특징으로 하고 있는 것이다.In the present invention, the concentration of the zinc chloride in the chloride plating bath is 100-150 g / l, or the potassium chloride and ammonium chloride, which are conductive additives, are added alone or mixed to the zinc chloride concentration to increase the concentration of the conductive additive to 100 g / l. By less than l, the precipitation overvoltage of zinc ions is increased, thereby decreasing the growth rate of zinc crystals, which in turn reduces the size of zinc crystals, and also the preferred orientation of zinc base surface parallel to the surface is 6 or more. It is characterized by increasing the gloss by increasing.

또한, 본 발명은 염화물계 도금욕을 사용하고, 연속 전기아염도금하는 전기아연도금강판의 제조방법이면 충분히 실시가능하지만, 보다 바람직하게는 염화물계 도금욕을 사용하고, 통상의 도금조건인 pH를 3-7, 도금욕의 온도를 40-60℃로 하여 연속 전기아연도금하는 전기도금강판의 제조방법에서 실시되는 것이 더욱 우수한 효과를 나타낸다.In addition, the present invention can be sufficiently carried out using a chloride plating bath, and a method of producing an electrogalvanized steel sheet subjected to continuous electroplating, but more preferably using a chloride plating bath, and the pH is a normal plating condition. 3-7, the temperature of the plating bath is 40-60 ℃ to be carried out in the method of producing an electroplated steel sheet of continuous electro-galvanized shows a more excellent effect.

본 발명에서 상기 염화아연의 농도를 100g/ℓ 미만으로 하면, 석출과전압이 너무 크기 때문에 도금층의 광택도는 우수하지만, 도금효율이 낮아 연속 도금설비에는 부적당하며, 또한 150g/ℓ 이상으로 하는 경우에는 도금효율은 우수하지만, 전착아연결정의 크기가 비교적 크고 아연기저면의 우선배향도가 낮아 도금층의 광택성이 떨어지는 문제점이 있으므로 염화아연의 농도는 100-150g/ℓ로 하는 것이 바람직하다.In the present invention, when the concentration of zinc chloride is less than 100 g / l, because the precipitation overvoltage is too high, the glossiness of the plating layer is excellent, but the plating efficiency is low, which is unsuitable for continuous plating equipment, and when it is 150 g / l or more. Although the plating efficiency is excellent, the zinc chloride concentration is preferably 100-150 g / L since the size of electrodeposited zinc crystal is relatively large and the preferred orientation of the zinc base is low, resulting in poor glossiness of the plating layer.

또한, 상기 전도보조제의 첨가량이 100g/ℓ 이상으로 첨가되는 경우, 도금효율은 우수하지만, 전착아연결정의 크기가 비교적 크고 우선배향도가 낮아 도금층의 광택도가 떨어지므로 전도보조제의 농도는 100g/ℓ 이하로 하는 것이 바람직하다.In addition, when the addition amount of the conductive support agent is more than 100g / ℓ, the plating efficiency is excellent, but the electrodeposited zinc crystal size is relatively large and the degree of preferential orientation is low, so the gloss of the plating layer is lowered, the concentration of the conductive aid 100g / ℓ It is preferable to set it as follows.

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

실시예Example

일반가전용 냉연강판을 하기 표 1과 같은 조성을 갖는 도금욕에서, 도금용액의 pH : 4.5, 용액온도 : 60℃, 도금액유속 : 1.5m/초 및 전류밀도 : 60A/dm2의 도금조건으로 연속 전기아연도금한 후, 도금된 강판에 대하여 도금효율(시간당 부착량), 도금층 우선배향도, 도금결정립 크기 및 표면광택도를 측정하고, 그 결과를 하기 표 1에 나타내었다.In the plating bath having the composition shown in Table 1, a cold rolled steel sheet for general home use, the plating solution pH: 4.5, the solution temperature: 60 ℃, the plating liquid flow rate: 1.5m / sec and the current density: 60A / dm 2 plating conditions continuous electricity After galvanizing, the plating efficiency (adhesive amount per hour), plating layer preferential orientation, plating grain size, and surface glossiness of the plated steel sheets were measured, and the results are shown in Table 1 below.

상기 우선배향도는 상기 식(1)을 통하여 구하였고, 상기 도금층 광택도는 디지털 광택계(digital gloss meter, SUGA사 제품)을 이용하여 입사각 60°로 측정하였다.The preferred orientation was obtained through Equation (1), and the glossiness of the plating layer was measured at an incident angle of 60 ° using a digital gloss meter (manufactured by SUGA).

상기 표 1에 나타난 바와같이 본 발명예(1-9)은 본 발명에 따라 조성된 도금욕에서 연속 전기아연도금한 경우로서, 음극에서 아연이온의 석출과전압이 증가하여, 이로 인해 아연결정의 성장속도가 감소되어 결정크기가 미세하고, 또한 표면에 평행한 아연기저면의 우선배향성이 6 이상으로 증가되어서 광택도가 17 이상으로 우수하고, 도금효율은 95% 이상이었지만, 본 발명에서 한정한 농도범위 미만인 비교예(1-3)의 경우에는 석출과전압이 너무 크기 때문에 도금층의 광택도는 우수하지만, 도금효율 95% 이하로 낮아 연속 도금설비에는 부적당하다는 것을 알 수 있다. 또한, 본 발명의 농도범위를 초과하는 비교예(4-9)의 경우에는 도금효율은 우수하지만, 전착아연결정의 크기가 비교적 크고 아연기저면의 우선배향율이 낮아 도금층의 광택성이 떨어짐을 알 수 있었다.As shown in Table 1, Example (1-9) of the present invention is a case of continuous electro-galvanizing in a plating bath formed according to the present invention, which increases the precipitation overvoltage of zinc ions in the cathode, thereby increasing the growth of zinc crystals. Although the speed was decreased, the crystal size was fine, and the preferred orientation of the zinc base surface parallel to the surface was increased to 6 or more, so that the glossiness was excellent at 17 or more, and the plating efficiency was 95% or more, but the concentration range defined in the present invention was limited. In the case of Comparative Example (1-3) which is less than, the precipitation overvoltage is too high, the gloss of the plating layer is excellent, but the plating efficiency is lower than 95%, it can be seen that it is not suitable for continuous plating equipment. In addition, in the case of Comparative Example (4-9) exceeding the concentration range of the present invention, the plating efficiency is excellent, but the electrodeposited zinc crystal is relatively large and the preferred orientation of the zinc base is low, so that the glossiness of the plating layer is deteriorated. Could.

상술한 바와같이, 본 발명은 염화물계 도금욕의 도금용액의 농도를 조절하여 아연도금강판의 광택성을 높이는 방법으로서, 그 실시에 있어서 간편하고, 또한 도금효율의 감소나 도금된 후 색상의 변화 및 균열이 발생되는 문제점이 없이 아연도금강판의 광택성을 현저하게 높일 수 있는 효과가 있는 것이다.As described above, the present invention is a method of increasing the glossiness of a galvanized steel sheet by adjusting the concentration of a plating solution of a chloride plating bath, which is simple in its implementation, and also reduces the plating efficiency or changes in color after plating. And there is an effect that can significantly increase the glossiness of the galvanized steel sheet without the problem of cracking.

Claims (2)

염화물계 도금욕을 사용하고, 통상의 도금조건인 pH를 3-7, 도금욕의 온도를 40-60℃로 하여 연속 전기아연도금하는 전기아연도금강판의 제조방법에 있어서, 상기 염화물계 도금욕중의 염화아연 농도가 100-150g/ℓ이 되도록 염화물계 도금욕을 조성하여 아연기저면의 우선배향도가 6 이상이 되도록 연속 전기아연도금하는 것을 특징으로 하는 표면광택성이 우수한 전기아연도금강판의 제조방법.In the method for producing an electro-galvanized steel sheet using a chloride plating bath, continuous electro-galvanizing at a pH of 3-7 and a plating bath temperature of 40-60 ° C., which are ordinary plating conditions, the chloride plating bath Preparation of an electro-zinc plated steel sheet having excellent surface gloss, characterized by forming a chloride plating bath so that the concentration of zinc chloride in the solution is 100-150 g / l and continuously electro-galvanizing so that the preferred orientation of the zinc base surface is 6 or more. Way. 염화물계 도금욕을 사용하고, 통상의 도금조건인 pH를 3-7, 도금욕의 온도를 40-60℃로 하여 연속 전기아연도금하는 전기아연도금강판의 제조방법에 있어서, 상기 염화물계 도금욕중의 염화아연 농도가 100-150g/ℓ이고, 상기 도금욕에 전도보조제로 염화칼륨 및 염화암모늄을 단독 또는 혼합 첨가하여 상기 전도보조제의 농도가 100g/ℓ 이하가 되도록 염화물계 도금욕을 조성하여 아연기저면의 우선배향도가 6 이상이 되도록 연속 전기아연도금하는 것을 특징으로 하는 표면광택성이 우수한 전기아연도금강판의 제조방법.In the method for producing an electro-galvanized steel sheet using a chloride plating bath, continuous electro-galvanizing at a pH of 3-7 and a plating bath temperature of 40-60 ° C., which are ordinary plating conditions, the chloride plating bath The zinc chloride concentration in the zinc chloride was 100-150 g / l, and the chloride-based plating bath was formed so that the concentration of the conduction aid was 100 g / l or less by adding or adding potassium chloride and ammonium chloride as the conduction aid to the plating bath. A method for producing an electro-zinc plated steel sheet having excellent surface glossiness, characterized by continuous electro-zinc plating so that the preferred orientation of the base surface is 6 or more.
KR1019930030259A 1993-12-28 1993-12-28 Method for manufacturing a electro-zinc plating steel sheets with an excellent surface brightness KR960008154B1 (en)

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