KR100579411B1 - Zn-Ni-W alloy electrodeposited steel sheets for good adhesion and corrosion resistance - Google Patents
Zn-Ni-W alloy electrodeposited steel sheets for good adhesion and corrosion resistance Download PDFInfo
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Abstract
본 발명은 가용성 양극을 사용하는 아연-니켈-텅스텐 합금 전기도금용액 및 이 용액을 이용한 아연-니켈-텅스텐 합금 전기도금강판의 제조방법에 관한 것으로서, 염화아연의 아연이온 몰농도: 0.5∼2.0 mol/liter, 염화니켈의 니켈이온 몰농도: 0.05∼0.4 mol/liter, 소디움 텅스테네이트의 텅스텐 이온 몰농도: 0.005~2.0 mmol/liter 및 염소이온의 몰 농도: 2.0∼9.0 mol/liter로 조성되는 것을 특징으로 하는 아연-니켈-텅스텐 합금 전기도금용액과 상기 아연-니켈-텅스텐 합금 전기도금용액의 온도를 40∼70℃, 전류밀도를 20 ∼ 180 A/d㎡ 및 상기 전기도금용액과 음극의 상대 유속을 0.5∼2.5m/sec.의 도금조건으로 전기도금하는 것을 특징으로 하는 아연-니켈-텅스텐 합금 전기도금강판의 제조방법으로써, 아연-니켈-텅스텐 합금도금의 내식성과 밀착성이 우수한 효과를 나타낸다.The present invention relates to a zinc-nickel-tungsten alloy electroplating solution using a soluble anode, and to a method for producing a zinc-nickel-tungsten alloy electroplating steel sheet using the solution. / liter, nickel ion molarity of nickel chloride: 0.05-0.4 mol / liter, tungsten ion molarity of sodium tungstenate: 0.005-2.0 mmol / liter and molar concentration of chlorine ion: 2.0-9.0 mol / liter Characterized in that the temperature of the zinc-nickel-tungsten alloy electroplating solution and the zinc-nickel-tungsten alloy electroplating solution is 40 ~ 70 ℃, the current density of 20 ~ 180 A / dm 2 and the electroplating solution and the cathode As a method of manufacturing a zinc-nickel-tungsten alloy electroplating steel sheet, the electroplating is performed under a plating condition of a relative flow rate of 0.5 to 2.5 m / sec., The effect of excellent corrosion resistance and adhesion of zinc-nickel-tungsten alloy plating is obtained. Indicated .
도금용액, 텅스텐, 합금전기도금, 밀착성, 내식성Plating solution, tungsten, alloy electroplating, adhesion, corrosion resistance
Description
본 발명은 가용성 양극을 사용하는 아연-니켈-텅스텐 합금 전기도금용액 및 이 용액을 이용한 아연-니켈-텅스텐 합금 전기도금강판의 제조방법에 관한 것이다.The present invention relates to a zinc-nickel-tungsten alloy electroplating solution using a soluble anode and a method for producing a zinc-nickel-tungsten alloy electroplating steel sheet using the solution.
일반적으로 철 위에 금속 도금을 하는 것은 옛날부터 방청, 장식 등을 위해서 많이 사용되어져 왔다. 특히 오늘날에는 강판의 내식성을 확보하기 위하여 아연 전기도금 방법이 개발되면서 가전, 자동차, 건설 등등의 분야에 널리 사용되어 오고 있다. 그러나 가혹한 분위기 하에서의 내식성을 확보하기 위해서는 아연 도금층의 두께를 더욱더 증가시켜야 함에 따라 이를 제조하는 비용의 증가는 물론 밀착성 및 가공성 등에 좋지 않은 영향을 주었다. 따라서 이러한 결점을 해결하기 위해서 아연-니켈 합금전기도금 방법이 개발되어 왔다.In general, metal plating on iron has been used for a long time for rust prevention and decoration. In particular, the zinc electroplating method has been developed to secure the corrosion resistance of the steel sheet has been widely used in the fields of home appliances, automobiles, construction and so on. However, in order to secure corrosion resistance under severe atmosphere, the thickness of the galvanized layer should be further increased, which has an adverse effect on adhesion and processability, as well as an increase in the cost of manufacturing the same. Therefore, zinc-nickel alloy electroplating method has been developed to solve this drawback.
이와 같은 아연-니켈 합금전기도금은 도금욕의 성분에 따라서 여러가지가 있으나, 그 중 산성 도금욕을 기본으로 한 도금재 생산 방식이 일반적으로 널리 사용되어 오고 있다. 산성욕에는 황화물욕이 기본이 되는 것과 염화물욕이 기본이 되는 것 등이 있다. 여기에서 염화물욕은 황화물욕에 비하여 전기 전도도가 우수하여 고 전류 밀도 도금이 가능할 뿐만 아니라 주로 용해성 양극을 사용함으로써 불용성 양극을 사용하는 황화물욕에 비하여 용액의 제어가 편리하고 비용이 적게 든다. 상기의 용해성 양극은 주로 아연과 니켈을 사용하며 일반적으로 아연이 약 85% 이상이다. 이와 같은 용해성 양극을 사용할 때는 아연 양극에 슬러지(sludge)나 이물질이 부착되지 않아야 양호한 도금층과 내식성을 확보할 수 있다.Such zinc-nickel alloy electroplating is various depending on the components of the plating bath, but the plating material production method based on the acid plating bath has been widely used. Acid baths include sulfide baths as the basis and chloride baths as the base. Here, the chloride bath has excellent electrical conductivity compared to the sulfide bath, which enables high current density plating, and mainly uses a soluble anode, so that control of the solution is more convenient and less expensive than a sulfide bath using an insoluble anode. The soluble anode mainly uses zinc and nickel, and generally zinc is about 85% or more. When using such a soluble anode, a good plating layer and corrosion resistance can be secured when no sludge or foreign matter is attached to the zinc anode.
이상과 같은 아연-니켈 합금전기도금에 관한 공지 기술로는 일본특허공개 소63-130794호의 아연니켈계 합금전기도금강판의 제조방법과 일본특허공개 평3-52551호의 아연-니켈계 합금전기도금의 고전류 도금방법 및 미국특허 US-4834845호의 아연-니켈 전기도금강판등이 있으나 이들은 아연-니켈합금도금에서의 니켈의 합금비가 10-18%정도로 높아야 내식성이 양호한 것으로 나타남으로써 도금욕에서 니켈의 높은 농도에 의하여 비용이 많이 들뿐만 아니라 밀착성이 좋지않은 결과를 나타내었다. 이에 본 발명자들은 연구와 실험을 거듭 수행한 결과 아연-니켈-텅스텐 합금 도금강판은 낮은 농도의 텅스텐을 첨가하고서도 상기 공지기술에 비해 Ni함량을 1/2이상 낮추어 내식성 및 밀착성이 오히려 양호해지는 결과를 얻었다.As a known technique for zinc-nickel alloy electroplating as described above, the manufacturing method of zinc-nickel alloy electroplating steel sheet of Japanese Patent Application Laid-Open No. 63-130794 and the zinc-nickel alloy electroplating of Japanese Patent Publication No. 3-52551 There are high current plating method and zinc-nickel electroplating steel sheet of US Pat. No. 4,834,845. However, they show good corrosion resistance when the alloy ratio of nickel in zinc-nickel alloy plating is about 10-18%. It is not only expensive but also poor adhesion. Accordingly, the inventors have repeatedly conducted studies and experiments, and the zinc-nickel-tungsten alloy plated steel sheet has a result that the Ni content is lowered by 1/2 or more compared with the above-described known technology even though low tungsten is added. Got it.
본 발명은 상기한 종래기술의 제반 문제점을 해결하기 위하여 염화아연과 염화니켈을 기본으로 하는 염화물욕 도금용액에 미량의 텅스텐을 첨가하고, 적정 도금조건으로 제어함으로써 도금층의 밀착성과 내식성이 양호한 아연-니켈-텅스텐 합금 전기도금용액 및 이를 이용한 아연-니켈-텅스텐 합금 전기도금강판의 제조방법을 제공하는 데 그 목적이 있다.
The present invention is to solve the above problems of the prior art zinc zinc chloride and nickel chloride-based chloride bath plating solution by adding a small amount of tungsten, and controlled by the appropriate plating conditions, zinc- An object of the present invention is to provide a nickel-tungsten alloy electroplating solution and a method of manufacturing a zinc-nickel-tungsten alloy electroplating steel sheet using the same.
상기 목적을 달성하기 위한 본 발명은, 염화아연의 아연이온 몰농도: 0.5∼2.0 mol/liter, 염화니켈의 니켈이온 몰농도: 0.05∼0.4 mol/liter, 소디움 텅스테네이트의 텅스텐 이온 몰농도: 0.005~2.0 mmol/liter 및 염소이온의 몰 농도: 2.0∼9.0 mol/liter로 조성되는 것을 특징으로 하는 아연-니켈-텅스텐 합금 전기도금용액을 제공한다.
또한, 염화아연의 아연이온 몰농도: 0.5∼2.0 mol/liter, 염화니켈의 니켈이온 몰농도: 0.05∼0.4 mol/liter, 소디움 텅스테네이트의 텅스텐 이온 몰농도: 0.005~2.0 mmol/liter 및 염소이온의 몰 농도: 2.0∼9.0 mol/liter로 조성되는 것을 특징으로 하는 아연-니켈-텅스텐 합금 전기도금용액의 온도를 40∼70℃, 전류밀도를 20 ∼ 180 A/d㎡ 및 상기 전기도금용액과 음극의 상대 유속을 0.5∼2.5m/sec.의 도금조건으로 전기도금하는 것을 특징으로 하는 아연-니켈-텅스텐 합금 전기도금강판의 제조방법을 제공한다.In order to achieve the above object, the present invention provides a zinc ion molar concentration of zinc chloride: 0.5 to 2.0 mol / liter, a nickel ion molar concentration of nickel chloride: 0.05 to 0.4 mol / liter, and a tungsten ion molar concentration of sodium tungsten: Provided is a zinc-nickel-tungsten alloy electroplating solution, characterized in that the composition of 0.005 ~ 2.0 mmol / liter and molar concentration of chlorine ion: 2.0 ~ 9.0 mol / liter.
The zinc ion molar concentration of zinc chloride: 0.5 to 2.0 mol / liter, the nickel ion nickel concentration of nickel chloride: 0.05 to 0.4 mol / liter, the tungsten ion molarity of sodium tungstenate: 0.005 to 2.0 mmol / liter and chlorine Molar concentration of ions: 40-70 DEG C, current density of 20-180 A / dm 2, and electroplating solution of zinc-nickel-tungsten alloy electroplating solution, characterized in that it is composed of 2.0-9.0 mol / liter. It provides a method for producing a zinc-nickel-tungsten alloy electroplating steel sheet characterized in that the electroplating under the plating conditions of 0.5 to 2.5m / sec.
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이하 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
[아연-니켈-텅스텐 합금 전기도금용액][Zinc-Nickel-Tungsten Alloy Electroplating Solution]
본 발명은 용해성 양극을 사용하여 염화아연과 염화니켈을 기본으로 하는 염화물욕 도금용액에 미량의 텅스텐을 첨가함으로써 도금층의 밀착성과 내식성을 향상 시키고자 하는 데 그 특징이 있다.The present invention is characterized by improving the adhesion and corrosion resistance of the plating layer by adding a small amount of tungsten to the chloride bath plating solution based on zinc chloride and nickel chloride using a soluble anode.
즉, 텅스텐을 0.005 mmol/liter에서 2.0 mmol/liter 첨가함에 따라 상기와 같은 도금용액에서 형성되는 도금층은 아연-니켈 합금도금 대비 내식성이 1.3 ~ 1.8배로 향상된다. 이러한 것은 텅스텐이 도금층에 함유됨으로서 도금층에 발생되는 핀홀 발생을 억제하는 것에 기인하는 것으로 사료된다.That is, by adding 2.0 mmol / liter of tungsten at 0.005 mmol / liter, the plating layer formed in the plating solution as described above has 1.3 to 1.8 times higher corrosion resistance than zinc-nickel alloy plating. This is considered to be due to suppression of pinhole generation generated in the plating layer by the inclusion of tungsten in the plating layer.
본 발명의 도금용액에 있어서, 염화아연의 아연이온 몰 농도가 0.5 mol/liter 미만인 경우에는 도금에 소요되는 총금속 이온의 부족으로 도금강판에 검게 그을리는 자국(burning)을 일으킬 수 있고, 2.0 mol/liter을 초과할 경우에는 도금층이 분말 형태의 도금이 되어서 밀착성이 떨어지게 된다. 따라서 상기 아연이온의 몰 농도는 0.5∼2.0 mol/liter로 제한하는 것이 바람직하다.In the plating solution of the present invention, when the zinc ion molar concentration of zinc chloride is less than 0.5 mol / liter, blacking of the plated steel sheet may occur due to a lack of total metal ions required for plating, and 2.0 When the mol / liter is exceeded, the plating layer is plated in powder form, resulting in poor adhesion. Therefore, the molar concentration of the zinc ion is preferably limited to 0.5 to 2.0 mol / liter.
상기 염화니켈의 니켈이온 몰농도가 0.05 mol/liter 미만에서는 도금층의 합금에서 니켈 함량이 떨어져서 내식성이 하락하며, 몰농도가 0.4 mol/liter을 초과하는 경우에는 도금층의 니켈 함량이 높아져 밀착성이 떨어진다. 따라서 상기 니켈이온 몰농도는 0.05∼0.4 mol/liter 범위로 제한하는 것이 바람직하다. When the nickel ion molar concentration of nickel chloride is less than 0.05 mol / liter, the nickel content of the plating layer is lowered to reduce corrosion resistance, and when the molar concentration exceeds 0.4 mol / liter, the nickel content of the plating layer is increased to decrease adhesion. Therefore, the nickel ion molar concentration is preferably limited to 0.05 to 0.4 mol / liter range.
상기 소디움 텅스테네이트의 텅스텐 이온이 0.005 mmol/liter 미만에서는 도금용액내에서의 텅스텐의 석출량이 너무작아 내식성이 떨어지며, 2.0 mmol/liter을 초과하면 밀착성이 감소하게 된다. 따라서 상기 텅스텐 이온은 0.005 mmol/liter에서 2.0 mmol/liter로 한정하는 것이 바람직하다.When the tungsten ion of the sodium tungstenate is less than 0.005 mmol / liter, the amount of tungsten in the plating solution is too small to reduce corrosion resistance, and when it exceeds 2.0 mmol / liter, the adhesion decreases. Therefore, the tungsten ion is preferably limited to 0.005 mmol / liter to 2.0 mmol / liter.
상기 염소이온의 몰농도가 2.0 mol/liter 미만에서는 전기 전도도의 감소로 인하여 버닝이 다량 발생하고, 9.0 mol/liter을 초과 하면 용해도 문제로 염소 이온이 석출된다. 따라서 상기 염소이온은 2.0∼9.0 mol/liter로 제한하는 것이 바람직하다.When the molarity of the chlorine ion is less than 2.0 mol / liter, a large amount of burning occurs due to a decrease in electrical conductivity, and when it exceeds 9.0 mol / liter, chlorine ions are precipitated due to solubility problems. Therefore, the chlorine ion is preferably limited to 2.0 to 9.0 mol / liter.
[아연-니켈-텅스텐 합금 전기도금강판의 제조방법][Manufacturing method of zinc-nickel-tungsten alloy electroplated steel sheet]
본 발명은 상기한 본 발명의 아연-니켈-텅스텐 합금 전기도금용액을 소지강판에 전기도금을 하여 도금층의 밀착성과 내식성을 향상시킬 수 있는 아연-니켈-텅스텐 합금 전기도금강판의 제조방법으로써 그 도금조건은 도금용액의 온도를 40 ∼ 70oC, 전류밀도를 20 ∼ 180A/dm2 및 도금용액과 음극의 상대 유속을 0.5 ∼ 2.5m/sec로 하는 것이 바람직하다.The present invention is a method of manufacturing a zinc-nickel-tungsten alloy electroplating steel sheet which can improve the adhesion and corrosion resistance of the plating layer by electroplating the zinc-nickel-tungsten alloy electroplating solution of the present invention described above. The conditions are preferably 40 to 70 ° C. for the plating solution, 20 to 180 A / dm 2 for the current density, and 0.5 to 2.5 m / sec for the relative flow rates of the plating solution and the cathode.
상기 도금용액의 온도가 40oC 미만에서는 도금층의 색상이 어둡고 도금층의 밀착성이 떨어져서 박리 현상이 나타난다. 도금용액의 온도가 70oC를 초과 되면 도금 줄무늬 현상이 심하며, 도금층의 광택이 없어지게 된다. When the temperature of the plating solution is less than 40 ° C., the color of the plating layer is dark and the adhesion of the plating layer is inferior, resulting in peeling phenomenon. If the temperature of the plating solution exceeds 70 o C plating phenomena are severe, the gloss of the plating layer is lost.
상기 전류밀도가 20A/dm2 미만이 되면 생산성의 감소로 비용이 증가되며, 180A/dm2 를 초과할 경우는 고전류밀도를 감당할 설비비의 증가로 역시 비용이 많이들게 된다.When the current density is less than 20A / dm 2 , the cost is increased by the decrease in productivity, and when the current density exceeds 180A / dm 2 , the cost is also increased due to the increase in the equipment cost to cover the high current density.
상기 도금용액과 음극의 상대 유속이 0.5m/sec 미만에서는 탄도금 즉, 버닝(burning)이 발생하며, 2.5m/sec이상을 초과할 경우는 균일한 유속을 얻기 힘들어져서 도금층이 불균일해지기 때문이다.When the relative flow rate of the plating solution and the negative electrode is less than 0.5m / sec, ballistic plating, that is, burning occurs, and when it exceeds 2.5m / sec, it becomes difficult to obtain a uniform flow rate and the plating layer becomes uneven. to be.
이하, 실시예를 통하여 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[실시예] EXAMPLE
냉연강판을 소지금속으로하여 하기 표1에 나타난 도금용액 조성을 가진 용액으로 전류밀도 60A/dm2, 온도 60oC, 유속 1.5m/sec에서 도금을 행하고 일본 지스 규격 제트-2371 으로 도금층의 내식성을 염수분무 후에 나타나는 붉은녹 발생을 기준으로 평가하였으며 도금 밀착성은 120o 구부린 뒤 Tape에 묻어나는 도금층의 박리량으로 측정하였다. 도금량은 30g/m2으로 도금하여 붉은 점녹의 발생 시간이 250시간 이상은 양호, 이하는 불량을 나타내었으며, 도금밀착성은 테이프에 도금층이 묻어나면 불량, 묻어나지않으면 양호로 판정하였다.The cold rolled steel is used as the base metal, and the plating solution composition shown in Table 1 is plated at a current density of 60 A / dm 2 , a temperature of 60 o C, and a flow rate of 1.5 m / sec. The red rust that appeared after the salt spray was evaluated based on the degree of plating adhesion. The adhesion was measured by the peeling amount of the plating layer deposited on the tape after bending at 120 ° . The plating amount was plated at 30 g / m 2, and the occurrence time of the red rust was more than 250 hours, which was good and the following was poor. Plating adhesion was judged to be poor when the plating layer was on the tape and good when not.
상기 표 1에서 알수 있듯이 본 발명의 도금용액 조성범위에 부합되는 발명예 1∼9는 도금의 품질특성을 나타내는 내식성과 밀착성에서 모두 양호한 결과를 나타내었다. 그러나 비교예 1과 2는 아연이온이 본 발명의 적정범위보다 적거나 초과 첨가됨으로써 도금 품질특성이 불량하게 나타났고, 또한 비교예 3은 니켈이온이 미량 첨가된 경우이고, 비교예 4는 니켈이온이 초과 첨가되고 텅스텐 이온이 미량첨가 되었으며, 비교예 5는 염소이온과 텅스텐 이온이 각각 초과 첨가된 것을 나타내었는 데, 이와 같이 비교예 3∼5에서도 도금 품질특성이 불량함을 알 수 있다.As can be seen from Table 1, Inventive Examples 1 to 9, which correspond to the plating solution composition range of the present invention, showed good results in both corrosion resistance and adhesion showing the quality characteristics of plating. However, Comparative Examples 1 and 2 showed poor plating quality characteristics due to the addition of less or more zinc ions than the proper range of the present invention, and Comparative Example 3 was a case where a small amount of nickel ions was added, and Comparative Example 4 was nickel ions. The excess was added and the tungsten ions were added in a small amount, Comparative Example 5 shows that the chlorine ions and tungsten ions are added in excess, respectively, it can be seen that the plating quality characteristics are also poor in Comparative Examples 3 to 5.
상술한 바와 같이 본 발명은 염화물계의 도금용액에 있어서 도금용액의 조성 및 도금조건을 적정하게 조정함으로써 아연-니켈-텅스텐 합금도금의 내식성과 밀착성이 우수한 효과를 나타낸다.As described above, the present invention exhibits an excellent effect of corrosion resistance and adhesion of zinc-nickel-tungsten alloy plating by appropriately adjusting the composition and plating conditions of the plating solution in the chloride plating solution.
Claims (2)
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56293A (en) * | 1979-06-18 | 1981-01-06 | Toyo Kohan Co Ltd | Production of dark color zinc electroplated steel plate |
| JPS57114686A (en) * | 1981-01-07 | 1982-07-16 | Toyo Kohan Co Ltd | Manufacture of bright and composite zinc electroplated steel plate |
| JPH07292491A (en) * | 1994-04-21 | 1995-11-07 | Hitachi Cable Ltd | High corrosion resistant plating film and plating liquid |
| KR960006597A (en) * | 1994-07-28 | 1996-02-23 | 이형도 | On-Screen Display of Cable Broadcast Converter |
| JP2001226795A (en) * | 1999-12-10 | 2001-08-21 | Nippon Denkai Kk | Roughening treated copper foil and producing method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56293A (en) * | 1979-06-18 | 1981-01-06 | Toyo Kohan Co Ltd | Production of dark color zinc electroplated steel plate |
| JPS57114686A (en) * | 1981-01-07 | 1982-07-16 | Toyo Kohan Co Ltd | Manufacture of bright and composite zinc electroplated steel plate |
| JPH07292491A (en) * | 1994-04-21 | 1995-11-07 | Hitachi Cable Ltd | High corrosion resistant plating film and plating liquid |
| KR960006597A (en) * | 1994-07-28 | 1996-02-23 | 이형도 | On-Screen Display of Cable Broadcast Converter |
| JP2001226795A (en) * | 1999-12-10 | 2001-08-21 | Nippon Denkai Kk | Roughening treated copper foil and producing method therefor |
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