KR20200054550A - Liquefaction reagent composition for plating layer of nickel plated steel sheet, and analyzing method of plating layer of nickel plated steel sheet using thereof - Google Patents
Liquefaction reagent composition for plating layer of nickel plated steel sheet, and analyzing method of plating layer of nickel plated steel sheet using thereof Download PDFInfo
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Abstract
Description
본 발명은 니켈도금강판의 도금층 분석용 용해액 조성물 및 이를 이용하여 니켈도금강판의 도금층에 포함된 니켈 함량의 분석 방법에 관한 것이다.The present invention relates to a solution composition for analyzing the plating layer of a nickel plated steel sheet and a method of analyzing the nickel content contained in the plating layer of a nickel plated steel sheet using the same.
최근 고강도 강판의 수요 증가와 더불어 자동차 부품 등의 용도로 쓰이는 강판에 대한 요구가 매우 엄격해져, 도금 물성뿐만 아니라 가공성이 우수한 제품이 요구되고 있다. 연속도금 라인에서 생산되는 도금강판의 경우, 성분 계와 도금층 두께, 도금 부착량에 따라 도금층의 물성과 가공성, 내식성이 결정되는데, 이때 일정 이상의 니켈을 함유하는 도금강판은 가공성에 있어서 중대한 취약점으로 나타나게 된다. Recently, along with the increasing demand for high-strength steel sheets, the demand for steel sheets used for automobile parts, etc. has become very strict, and thus products with excellent plating properties as well as processability are required. In the case of a plated steel sheet produced in a continuous plating line, the physical properties, processability, and corrosion resistance of the plated layer are determined according to the component system, the thickness of the plated layer, and the amount of plated deposits. .
따라서 도금강판의 도금 부착량을 측정하기 위하여 도금강판의 시편 채취 후 합금 금속화된 도금층을 액상화하고, 분석 기기를 통하여 니켈을 정량 측정함으로써 단위면적당 니켈도금 부착량을 산출한다. Therefore, in order to measure the plating adhesion amount of the plated steel sheet, after collecting the specimen of the plated steel sheet, the alloyed metallized plating layer is liquefied, and the nickel plating amount per unit area is calculated by quantitatively measuring nickel through an analysis device.
그러나, 종래의 도금층 분석용 용해액 조성물은 일반적으로 단일 산으로서, 니켈 합금 금속의 특성상 단일 산에는 초기 용해 시 환원금속이 생성되며, 환원금속 생성 후에는 도금층이 용해되지 않는다. 또한, 액상화된 니켈이 소지 금속에 다시 무전해 도금되는 특성으로 인하여 도금층이 전량 액상화되지 않는 문제가 있다. 이에, 도금층이 불완전 액상화되어, 액상화된 도금층의 니켈 함량 측정 시 오차가 발생하고, 도금 부착량 산술치가 신뢰 수준을 벗어나 있었다.However, the conventional solution for analyzing the plating layer is a single acid, and due to the properties of the nickel alloy metal, a single acid generates a reduced metal upon initial dissolution, and the plated layer does not dissolve after generating the reduced metal. In addition, due to the property that the liquefied nickel is electrolessly plated on the base metal again, there is a problem that the entire amount of the plating layer is not liquefied. As a result, the plating layer was incompletely liquefied, an error occurred when measuring the nickel content of the liquefied plating layer, and the arithmetic value of the plating adhesion amount was out of confidence.
상기와 같이 종래의 도금 부착량 측정 방법은 신뢰할 수 없으며, 특히 합금 도금층이 완전히 용해되지 않은 시료를 사용함으로써, 도금 부착량 적중률 향상이 어려운 문제가 있었다. As described above, the conventional method for measuring the amount of plating adhesion is unreliable, and in particular, by using a sample in which the alloy plating layer is not completely dissolved, there is a problem that it is difficult to improve the plating adhesion amount hit ratio.
따라서, 본 발명의 목적은 니켈도금강판의 도금 부착량을 측정함에 있어서, 분석기기에서 정량 분석이 가능하도록 고체상 합금 도금층을 전량 액상화하여 도금 부착량을 정확하게 산출할 수 있도록 하는 니켈도금강판 도금층 분석용 용해액 조성물을 제공하는 것이다. Accordingly, an object of the present invention is to measure the amount of plating on a nickel-plated steel sheet, so that the solid-state alloy plating layer is liquefied in a total amount to enable quantitative analysis in an analyzer, so that the solution for analyzing the plating layer of a nickel-plated steel sheet can be accurately calculated. It is to provide a composition.
본 발명의 다른 목적은 일반적인 방법으로 도금층 액상화 작업 중 도금층이 용해되지 않는 문제와, 액상화 된 도금층에서 니켈원소가 소지철에 무전해 도금되는 특성으로 인하여 완전하지 않는 액상화로 정확한 정량 측정이 불가한 문제를 극복하기 위해 니켈도금강판 도금층 분석용 용해액 조성물을 이용한 니켈도금강판 도금층 분석 방법을 제공하는 것이다.Another object of the present invention is the problem that the plating layer does not dissolve during the liquefaction of the plating layer by a general method, and the accurate quantitative measurement is not possible due to the incomplete liquefaction due to the property that the nickel element is electrolessly plated on the iron in the liquefied plating layer. In order to overcome the above, it is to provide a method for analyzing a plated layer of a nickel plated steel sheet using a solution composition for analysis of a plated layer of a nickel plated steel sheet.
본 발명의 일 실시예에 따르면, 도금층 분석용 용해액 조성물에 대하여 염산 30 내지 60 부피%, 과산화수소 1 내지 25 부피% 및 잔부 물을 포함하는 니켈도금강판 도금층 분석용 용해액 조성물을 제공한다.According to an embodiment of the present invention, a solution for analyzing a plated layer of a nickel plated steel sheet containing 30 to 60% by volume of hydrochloric acid, 1 to 25% by volume of hydrogen peroxide and the remainder water is provided with respect to the solution composition for analyzing the plating layer.
본 발명의 다른 실시예에 따르면, 도금층 분석용 용해액 조성물에 대하여 염산 30 내지 60 부피%, 과산화수소 1 내지 25 부피% 및 잔부 물을 포함하는 용해액 조성물을 준비하는 용해액 조성물 준비 단계; 니켈도금강판의 도금층 표면에 과산화수소 수용액을 도포하여 활성 산화시키는 활성 산화 단계; 니켈도금강판을 용해액 조성물에 침지하여 도금층을 용해하는 도금층 용해 단계; 및 용해된 도금층으로부터 도금 부착량을 산출하는 분석 단계를 포함하는 니켈도금강판 도금층 분석 방법을 제공한다.According to another embodiment of the present invention, a solution composition preparation step of preparing a solution composition containing 30 to 60% by volume of hydrochloric acid, 1 to 25% by volume of hydrogen peroxide and the balance water with respect to the solution composition for analyzing the plating layer; An active oxidation step of active oxidation by applying an aqueous hydrogen peroxide solution on the surface of the plating layer of the nickel plated steel sheet; A plating layer dissolving step of immersing the nickel plated steel sheet in a solution composition to dissolve the plating layer; And an analytical step of calculating a plating adhesion amount from the dissolved plating layer.
상기 활성 산화 단계에서 사용되는 과산화수소 수용액의 농도는 1 내지 30 부피%이며, 과산화수소 수용액의 도포 시간은 1 내지 20초이다. The concentration of the aqueous hydrogen peroxide solution used in the active oxidation step is 1 to 30% by volume, and the application time of the aqueous hydrogen peroxide solution is 1 to 20 seconds.
상기 도금층 용해 단계에서, 니켈도금강판은 용해액 조성물에 5 내지 25분 동안 침지된다.In the plating layer dissolving step, the nickel plated steel sheet is immersed in the solution composition for 5 to 25 minutes.
상기 분석 단계에서 도금 부착량은 유도결합 플라즈마 발광분광분석 또는 원자흡광광도법에 의해 산출된다.In the above analysis step, the plating adhesion amount is calculated by inductively coupled plasma emission spectrometry or atomic absorption spectrometry.
본 발명의 니켈도금강판 도금층 분석용 용해액 조성물을 이용하여 니켈도금강판의 도금층을 전량 액상화함으로써, 분석기기를 통하여 도금층에 포함된 원소를 정량 분석할 수 있다. 이러한 결과로부터 니켈도금강판의 도금층 두께, 도금 부착량을 산출할 수 있으며, 결과적으로 보다 정밀하고 효율적으로 도금강판 생산, 품질관리가 가능해진다.By liquefying the entire amount of the plating layer of the nickel-plated steel sheet using the solution composition for analyzing the plating layer of the nickel-plated steel sheet of the present invention, it is possible to quantitatively analyze the elements included in the plating layer through an analyzer. From these results, it is possible to calculate the plating layer thickness and plating adhesion of the nickel plated steel sheet, and as a result, it becomes possible to more accurately and efficiently produce and quality control the plated steel sheet.
도 1은 본 발명의 도금층 분석용 용해액 조성물을 사용하여 니켈도금강판의 도금층을 전량 액상화한 용액(도 1A) 및 도금층이 전량 제거된 소지금속(도 1B)이다.
도 2는 종래의 도금층 분석용 용해액 조성물을 사용하여 니켈도금강판의 도금층이 일부 액상화된 용액(도 2A) 및 용해액 조성물에 침지 후 니켈이 무전해 도금된 소지금속(도 2B)이다.1 is a solution obtained by liquefying the entire plating layer of a nickel plated steel sheet using the solution composition for analyzing the plating layer of the present invention (FIG. 1A) and a base metal from which the plating layer is entirely removed (FIG. 1B).
2 is a base metal plated with nickel electrolessly plated after immersion in a solution (FIG. 2A) and a solution in which the plating layer of the nickel plated steel sheet is partially liquefied using a conventional solution for analyzing a plating layer (FIG. 2B).
이하, 본 발명의 바람직한 실시 형태를 설명한다. 그러나 본 발명의 실시 형태는 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 이하 설명하는 실시 형태로 한정되는 것은 아니다.Hereinafter, preferred embodiments of the present invention will be described. However, embodiments of the present invention may be modified in various other forms, and the scope of the present invention is not limited to the embodiments described below.
본 발명의 도금층 분석용 용해액 조성물은, 도금층 분석용 용해액 조성물 대비 염산 30 내지 60 부피%, 과산화수소 1 내지 25 부피%를 포함하고, 잔부는 물이다. 상기 조성물에서 염산, 과산화수소가 상기 범위로 배합되는 경우에 도금층이 전량 액상화 된다. 본 발명에서 도금층은 아연-알루미늄-니켈 합금을 포함하는 것일 수 있다. The solution composition for analyzing the plating layer of the present invention contains 30 to 60% by volume of hydrochloric acid and 1 to 25% by volume of hydrogen peroxide, and the remainder is water compared to the solution for analyzing the plating layer. When the hydrochloric acid and hydrogen peroxide are blended in the above range in the composition, the plating layer is liquefied. In the present invention, the plating layer may include a zinc-aluminum-nickel alloy.
상기 도금층 분석용 용해액 조성물을 이용하면 도금강판 시편에서 도금층만을 선택적으로 액상화 시킬 수 있고, 특히 용해된 니켈 이온이 소지 금속 면에 무전해 도금되지 않으므로 도금층에 포함된 금속 전량을 정량 측정하여 도금 부착량을 정확하게 산출할 수 있다.When the solution composition for analyzing the plating layer is used, only the plating layer can be selectively liquefied in the specimen of the plated steel sheet. Particularly, since the dissolved nickel ions are not electrolessly plated on the surface of the metal, the amount of metal contained in the plating layer is quantitatively measured to deposit the amount Can calculate accurately.
본 발명의 용해액 조성물에서 염산은 도금층의 산화니켈을 용해시키기 위한 것이다. 상기 염산의 함량이 용해액 조성물 대비 30 부피% 미만이면 도금층의 니켈을 충분히 용해시키지 못하므로 바람직하지 않으며, 60 부피%를 초과하면 과포화에 의한 이온교환이 활성화되지 않아 도금층이 충분히 액상화되지 않으므로 바람직하지 않다.In the solution composition of the present invention, hydrochloric acid is for dissolving nickel oxide in the plating layer. If the content of the hydrochloric acid is less than 30% by volume compared to the solution composition, it is not preferable because nickel of the plating layer is not sufficiently dissolved, and if it exceeds 60% by volume, the ion exchange by supersaturation is not activated and the plating layer is not sufficiently liquefied. not.
한편, 본 발명의 용해액 조성물에서 과산화수소는 도금층의 금속화합물과 염산이 반응하여 생성되는, 산에 불용성인 금속 환원물질 생성을 억제시키고, 니켈산화물을 생성하기 위한 것이다. 따라서, 상기 과산화수소의 함량이 1 부피% 미만이면 니켈 산화물 생성을 억제시킬 수 없으므로 소지 금속 면에 니켈이 무전해 도금 될 수 있어 바람직하지 않다. 반면, 과산화수소가 25 부피%를 초과하면 소지 금속과 과산화수소의 화학반응으로 침전물을 생성하여 액상화 용액 특성을 상실하므로 도금층 정량 분석에 오차가 발생할 수 있다.On the other hand, in the solution composition of the present invention, hydrogen peroxide is intended to suppress the formation of a metal reducing material insoluble in acid, which is generated by the reaction of a metal compound and hydrochloric acid in the plating layer, and to produce nickel oxide. Therefore, if the content of the hydrogen peroxide is less than 1% by volume, it is not preferable because nickel oxide cannot be suppressed, so nickel can be electrolessly plated on the surface of the metal. On the other hand, if the hydrogen peroxide exceeds 25% by volume, the chemical reaction of the metal and hydrogen peroxide creates a precipitate, which results in loss of the liquefaction solution properties, which may cause errors in the quantitative analysis of the plating layer.
상기 용해액 조성물을 미리 혼합하는 경우 염산과 과산화수소의 화학반응으로 인하여 도금층 용해 성능이 저하될 수 있으므로, 도금층의 액상화 반응 직전에 혼합하는 것이 바람직하다.When the solution mixture is pre-mixed, the plating layer dissolution performance may be reduced due to the chemical reaction of hydrochloric acid and hydrogen peroxide, so it is preferable to mix immediately before the liquefaction reaction of the plating layer.
본 발명의 도금층 분석 방법은, 도금층 분석용 용해액 조성물 대비 염산 30 내지 60 부피%, 과산화수소 1 내지 25 부피%를 포함하고, 잔부는 물인 용해액 조성물을 준비하는 용해액 조성물 준비 단계; 니켈도금강판의 도금층을 과산화수소를 이용하여 활성 산화시키는 활성 산화 단계; 활성화된 도금층을 용해액 조성물을 이용하여 용해하는 도금층 용해 단계; 및 용해된 도금층으로부터 도금 부착량을 산출하는 분석 단계를 포함한다. The plating layer analysis method of the present invention includes 30 to 60% by volume of hydrochloric acid and 1 to 25% by volume of hydrogen peroxide compared to the solution composition for analyzing the plating layer, and the preparation of the solution composition for preparing the solution composition, the balance being water; An active oxidation step of actively oxidizing the plating layer of the nickel plated steel sheet using hydrogen peroxide; A plating layer dissolving step of dissolving the activated plating layer using a solution composition; And an analysis step of calculating the plating adhesion amount from the dissolved plating layer.
상기 용해액 조성물 준비 단계에서는 도금층 분석용 용해액 조성물 대비 염산 30 내지 60 부피%, 과산화수소 1 내지 25 부피%를 포함하고, 잔부는 물인 용해액 조성물을 제조하는 단계로서, 염산, 과산화수소가 상기 범위로 배합되는 경우에 도금층이 전량 액상화 된다.In the preparation step of the solution composition, 30 to 60% by volume of hydrochloric acid and 1 to 25% by volume of hydrogen peroxide compared to the solution composition for analysis of the plating layer are prepared, and the remainder is water, wherein the solution composition is hydrochloric acid and hydrogen peroxide. When blended, the entire plating layer is liquefied.
이후 활성 산화 단계에서는 농도가 1 내지 30 부피%인 과산화수소 수용액을 이용하여 니켈도금강판의 도금층을 활성 산화시킨다. 과산화수소 수용액의 농도가 1 부피% 미만이면 도금층이 산화되지 않으며, 30 부피%를 초과하면 도금층과의 극렬한 반응으로 도금층 용해액 포집 용기 밖으로 산화니켈 용액이 튀는 문제가 있어 바람직하지 않다. Thereafter, in the active oxidation step, the plating layer of the nickel plated steel sheet is actively oxidized using an aqueous hydrogen peroxide solution having a concentration of 1 to 30% by volume. If the concentration of the aqueous hydrogen peroxide solution is less than 1% by volume, the plating layer is not oxidized, and if it exceeds 30% by volume, there is a problem in that the nickel oxide solution splashes out of the plating layer solution collection container due to intense reaction with the plating layer.
본 발명의 활성 산화 단계의 반응식은 하기 식(1)과 같다.The reaction formula of the active oxidation step of the present invention is as the following formula (1).
H2O2 + Ni → H2O + NiO + O2 식(1)H 2 O 2 + Ni → H 2 O + NiO + O 2 Expression (1)
도금층에 포함된 금속 상태의 니켈은 과산화수소 수용액에 의해 활성 산화되어 산화 니켈이 되며, 상기 산화 니켈은 이후 도금층 용해 단계에서 염산과 반응하여 니켈 이온 상태로 용해된다.The nickel in the metal state included in the plating layer is activated and oxidized by an aqueous hydrogen peroxide solution to become nickel oxide, and the nickel oxide is then dissolved in a nickel ion state by reacting with hydrochloric acid in the plating layer dissolving step.
상기 활성 산화 단계에서는 과산화수소 수용액을 도금층 표면에 1 내지 20초간 도포하여 도금층을 활성 산화 시킨다. 과산화수소 수용액 도포 시간이 1초 미만이면, 도금층이 충분히 활성 산화되지 않으며, 20초를 초과하여 과산화수소 수용액 도포 시 도금층과의 극렬한 반응으로 도금층 용해액 포집 용기 밖으로 산화니켈 용액이 튀는 문제가 있다.In the active oxidation step, an aqueous hydrogen peroxide solution is applied to the surface of the plating layer for 1 to 20 seconds to activate the plating layer. If the application time of the aqueous hydrogen peroxide solution is less than 1 second, the plating layer is not sufficiently active oxidized, and when the aqueous hydrogen peroxide solution is applied for more than 20 seconds, there is a problem that the nickel oxide solution splashes out of the plating layer solution collection container due to intense reaction with the plating layer.
도금층 용해 단계에서는 활성 산화된 도금층을 용해액 조성물을 이용하여 용해한다. 활성 산화 단계에서 생성된 산화 니켈과 염산이 반응하여 니켈 이온이 생성되며, 반응식은 하기 식(2)와 같다.In the plating layer dissolving step, the active oxidized plating layer is dissolved using a solution composition. Nickel ions are generated by the reaction of nickel oxide and hydrochloric acid generated in the active oxidation step, and the reaction formula is shown in the following formula (2).
NiO + 2H+ → Ni2+ + H2O 식(2)NiO + 2H + → Ni 2+ + H 2 O formula (2)
상기 단계에서 니켈도금강판을 용해액에 5 내지 25분 동안 침지하며, 침지 시간이 5분 미만이면 도금층이 충분히 용해되지 않아 도금층 정량 분석시 오차가 발생한다. 한편, 침지 시간이 25분을 초과하면 소지 금속이 용해되어 산화철 침전물이 생성되는 점에서 바람직하지 않다.In the above step, the nickel plated steel sheet is immersed in the solution for 5 to 25 minutes, and if the immersion time is less than 5 minutes, the plating layer is not sufficiently dissolved and an error occurs during quantitative analysis of the plating layer. On the other hand, when the immersion time exceeds 25 minutes, it is not preferable in that a metal oxide is dissolved and a precipitate of iron oxide is formed.
도금 부착량 분석 단계에서는 유도결합 플라즈마(inductively coupled plasma) 발광분광분석법 또는 원자흡광광도법을 이용하여 도금층 액상화 용액에 포함된 니켈, 아연, 알루미늄 등 금속의 함량을 측정한다. 상기 유도결합 플라즈마 발광분광분석법 또는 원자흡광광도법을 이용하면, 도금층이 용해된 용액 내 각 금속 원소별 질량을 측정할 수 있으며, 상기 측정된 값을 도금층 면적으로 나누면 단위면적당 도금 부착량을 알 수 있다.In the plating adhesion analysis step, the content of metals such as nickel, zinc, and aluminum contained in the liquefaction solution of the plating layer is measured using an inductively coupled plasma emission spectrometry or atomic absorption spectrometry. If the inductively coupled plasma emission spectrometry or atomic absorption spectrometry is used, the mass of each metal element in the solution in which the plating layer is dissolved can be measured. If the measured value is divided by the plating layer area, the plating adhesion amount per unit area can be known.
실시예Example
이하, 본 발명의 실시예에 대해 상세히 설명한다. 하기 실시예는 본 발명의 이해를 위한 것일 뿐, 본 발명을 한정하는 것은 아니다.Hereinafter, embodiments of the present invention will be described in detail. The following examples are only for understanding the present invention and are not intended to limit the present invention.
1. 실시예 11. Example 1
강판 상에 Ni 사전도금을 500mg/m2을 실시하고, 환원 분위기에서 소둔한 후 Al 0.13 질량%의 Zn 도금욕에 침지하여 편면기준 부착량 60g/m2의 아연도금강판을 제조하였다. 상기 아연도금강판을 가로 80 mm, 세로 80 mm로 절단하여 시편을 만들고, 일정면적이 되도록 제작된 유리를 고무패킹을 이용하여 시편과 유리기구를 밀착하여 클립으로 고정한다. 도금강판 표면에 농도가 30 부피%인 과산화수소 수용액 5 ml를 5 초간 도포하여 도금층을 활성 산화 시킨 후 본 발명에서 기술한 도금층 분석용 용해액 조성물 20ml(염산 10 ml, 과산화수소 3 ml, 물 7ml 포함)를 투입하여 10분 후 100 ml 플라스크에 포집하고, 수세용액으로 전량 플라스크 표 선을 맞춘다. 그 후, 용액을 유도결합플라즈마 발광분광분석기기에서 니켈, 아연, 알루미늄 원소를 정량 분석하여 도금 부착량을 산출 하였다.500 mg / m 2 of Ni pre-plating was performed on the steel sheet, and then annealed in a reducing atmosphere, and then immersed in a Zn plating bath of 0.13 mass% Al to prepare a galvanized steel sheet having a single-sided adhesion amount of 60 g / m 2 . The galvanized steel sheet is cut into a width of 80 mm and a length of 80 mm to make a specimen, and a glass made to be a certain area is fixed with a clip by closely bonding the specimen and glass mechanism using a rubber packing. 5 ml of an aqueous hydrogen peroxide solution having a concentration of 30% by volume on the surface of the plated steel sheet was coated for 5 seconds to oxidize the plating layer, and then 20 ml of the solution composition for analyzing the plating layer described in the present invention (including 10 ml of hydrochloric acid, 3 ml of hydrogen peroxide, and 7 ml of water) After 10 minutes of inputting, it was collected in a 100 ml flask, and the whole flask was lined with a washing solution. Thereafter, the solution was quantitatively analyzed for nickel, zinc, and aluminum elements in an inductively coupled plasma luminescence spectroscopy apparatus to calculate plating adhesion.
상기 도금층을 용해시킨 후 플라스크에 포집한 용액은 도 1(A)에서 볼 수 있듯이 침전물 없이 도금층이 전량 액상화된 상태임을 알 수 있다. 도금층이 용해된 후 소지금속 표면 상태는, 도 1(B)와 같이 소지금속만 노출되어 있어 도금층은 전량 용해되고 소지금속에 니켈이 재흡착되는 반응이 없다는 것을 알 수 있다. After dissolving the plating layer, the solution collected in the flask can be seen that the plating layer is completely liquefied without a precipitate as shown in FIG. 1 (A). After the plating layer is dissolved, it can be seen that the surface state of the base metal is only exposed to the base metal as shown in FIG. 1 (B), so that the plating layer is completely dissolved and there is no reaction in which nickel is re-adsorbed to the base metal.
따라서, 도금층에 포함된 금속이 완전하게 이온으로 액상화된 시료를 이용하면, 유도결합플라즈마 발광분광분석기기를 이용하여 일반적인 분석방법으로 도금 원소별로 정량 분석하여 부착량을 산출할 수 있다.Therefore, when a sample in which the metal contained in the plating layer is completely liquefied with ions is used, the amount of adhesion can be calculated by quantitative analysis for each plating element by a general analysis method using an inductively coupled plasma emission spectrometry.
2. 비교예 1~32. Comparative Examples 1 to 3
실시예 1과 동일한 방법으로 제조된 아연도금강판에 농도가 30 부피%인 과산화수소 수용액 5 ml를 5 초간 도포하여 도금층을 활성 산화 시킨 후, 하기 표 1에 기재된 도금층 분석용 용해액 조성물을 투입하여 아연도금강판의 도금 부착량을 산출 하였다. After applying 5 ml of an aqueous hydrogen peroxide solution having a concentration of 30% by volume to the galvanized steel sheet prepared in the same manner as in Example 1 for 5 seconds, the plated layer was subjected to active oxidation. The plating adhesion amount of the plated steel sheet was calculated.
상기 실시예 1 및 비교예 1~3에서 산출된 도금 부착량을 표 2에 나타내었다.Table 2 shows the plating adhesion amounts calculated in Example 1 and Comparative Examples 1 to 3.
(g/m2)Ni adhesion amount
(g / m 2 )
(g/m2)Zn adhesion amount
(g / m 2 )
(g/m2)Al adhesion amount
(g / m 2 )
(g/m2)Plating adhesion
(g / m 2 )
실시예 1에서 측정된 도금 부착량은 58.645g/m2로, 실제 도금 부착량인 60g/m2에 가장 가까운 것을 알 수 있다. 반면, 비교예 1 내지 3의 경우, 도금 실시예 1의 도금 부착량 측정 결과에 비해 부착량 측정 오차가 크게 나타났으며, 이는 도금층 분석용 용해액 조성물이 강판 도금층을 전량 용해하지 못하였기 때문이다.The exemplary coating weight measured in Example 1, it can be seen that the closest to 58.645g / m 2, the actual coating weight of 60g / m 2. On the other hand, in Comparative Examples 1 to 3, the deposition amount measurement error was larger than the plating deposition amount measurement result of the plating example 1, because the solution composition for analyzing the plating layer did not completely dissolve the steel plate plating layer.
3. 비교예 43. Comparative Example 4
아연-알루미늄-니켈 도금강판을 가로 80 mm, 세로 80 mm로 절단하고 시편을 일정면적이 되도록 제작된 유리를 고무패킹을 이용하여 시편과 유리기구를 밀착하고 클립으로 고정한다. HNO3:H2O=1:10 용액 30ml 투입하여 2시간 용해 후 100 ml 플라스크에 포집하고 수세용액으로 전량 플라스크 표 선을 맞춘다. The zinc-aluminum-nickel plated steel sheet is cut into a width of 80 mm and a length of 80 mm, and the glass made so that the specimen is a certain area is brought into close contact with the specimen and the glass mechanism using rubber packing and fixed with clips. 30 ml of HNO 3 : H 2 O = 1: 10 solution was dissolved for 2 hours, collected in a 100 ml flask, and the whole flask was lined with a washing solution.
그 후, 용액을 유도결합플라즈마 발광분광분석기기에서 니켈, 아연, 알루미늄 원소를 정량 분석하였다. 도 2(A)에서 보듯이 불완전 용해와 침전 생성으로 인하여 전량 액상화 되지 않으며, 도 2(B)와 같이 니켈의 전기화학 특성 때문에 도금층 용해 후 소지 금속에 니켈이 무전해 도금되는 현상이 발생하였다.Subsequently, the solution was quantitatively analyzed for nickel, zinc, and aluminum elements in an inductively coupled plasma emission spectrometer. As shown in FIG. 2 (A), the entire amount is not liquefied due to incomplete dissolution and precipitation, and due to the electrochemical properties of nickel as shown in FIG. 2 (B), nickel was electrolessly plated on the base metal after dissolving the plating layer.
Claims (6)
Dissolved liquid composition for analyzing the plating layer of a nickel-plated steel sheet containing 30 to 60% by volume of hydrochloric acid, 1 to 25% by volume of hydrogen peroxide, and the remainder of the solution.
니켈도금강판의 도금층 표면에 과산화수소 수용액을 도포하여 활성 산화시키는 활성 산화 단계;
니켈도금강판을 용해액 조성물에 침지하여 도금층을 용해하는 도금층 용해 단계; 및
용해된 도금층으로부터 도금 부착량을 산출하는 분석 단계를 포함하는 니켈도금강판 도금층 분석 방법.
A solution composition preparation step of preparing a solution composition containing 30 to 60% by volume of hydrochloric acid, 1 to 25% by volume of hydrogen peroxide, and the balance water relative to the solution composition for analysis of the plating layer;
An active oxidation step of active oxidation by applying an aqueous hydrogen peroxide solution on the surface of the plating layer of the nickel plated steel sheet;
A plating layer dissolving step of immersing the nickel plated steel sheet in a solution composition to dissolve the plating layer; And
Nickel plated steel plate plating layer analysis method comprising an analysis step of calculating the amount of plating adhesion from the molten plating layer.
상기 활성 산화 단계에서 사용되는 과산화수소 수용액의 농도는 1 내지 30 부피%인 것을 특징으로 하는 니켈도금강판 도금층 분석 방법.
According to claim 2,
Nickel plated steel plate plating layer analysis method characterized in that the concentration of the aqueous hydrogen peroxide solution used in the active oxidation step is 1 to 30% by volume.
상기 활성 산화 단계에서 과산화수소 수용액의 도포 시간은 1 내지 20초인 것을 특징으로 하는 니켈도금강판 도금층 분석 방법.
According to claim 2,
The plating method of the nickel-plated steel sheet is characterized in that the application time of the aqueous hydrogen peroxide solution in the active oxidation step is 1 to 20 seconds.
상기 도금층 용해 단계에서, 니켈도금강판은 용해액 조성물에 5 내지 25분 동안 침지되는 것을 특징으로 하는 니켈도금강판 도금층 분석 방법.
According to claim 2,
In the step of dissolving the plating layer, the nickel-plated steel sheet plating layer analysis method characterized in that the immersion in the solution composition for 5 to 25 minutes.
상기 분석 단계에서 도금 부착량은 유도결합 플라즈마 발광분광분석 또는 원자흡광광도법에 의해 산출되는 니켈도금강판 도금층 분석 방법.
According to claim 2,
The plating deposition amount in the analysis step is a method of analyzing a plated layer of a nickel plated steel sheet calculated by inductively coupled plasma emission spectrometry or atomic absorption spectrometry.
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| JPH10267918A (en) * | 1997-03-27 | 1998-10-09 | Nippon Steel Corp | Solution for chemical analysis of zinc-iron alloy group 2-layer plated steel board, and chemical analysis method using it |
| JP2001174452A (en) * | 1999-12-21 | 2001-06-29 | Hitachi Chem Co Ltd | Method of analyzing electroless nickel-plated coating, and etching liquid used for its analysis |
| JP2008224423A (en) * | 2007-03-13 | 2008-09-25 | Fujitsu Ltd | Plating film separation method and analysis method of plating film separated thereby |
| JP2008232730A (en) * | 2007-03-19 | 2008-10-02 | Sumitomo Metal Mining Co Ltd | Quantification method of impurities in nickel plating film |
| JP2009079902A (en) * | 2007-09-25 | 2009-04-16 | Yazaki Corp | Quantitative analysis method of nickel or nickel alloy plating layer |
-
2018
- 2018-11-12 KR KR1020180137953A patent/KR102218457B1/en active IP Right Grant
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS535498B1 (en) | 1968-04-29 | 1978-02-28 | ||
| JPH10267918A (en) * | 1997-03-27 | 1998-10-09 | Nippon Steel Corp | Solution for chemical analysis of zinc-iron alloy group 2-layer plated steel board, and chemical analysis method using it |
| JP2001174452A (en) * | 1999-12-21 | 2001-06-29 | Hitachi Chem Co Ltd | Method of analyzing electroless nickel-plated coating, and etching liquid used for its analysis |
| JP2008224423A (en) * | 2007-03-13 | 2008-09-25 | Fujitsu Ltd | Plating film separation method and analysis method of plating film separated thereby |
| JP2008232730A (en) * | 2007-03-19 | 2008-10-02 | Sumitomo Metal Mining Co Ltd | Quantification method of impurities in nickel plating film |
| JP2009079902A (en) * | 2007-09-25 | 2009-04-16 | Yazaki Corp | Quantitative analysis method of nickel or nickel alloy plating layer |
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| KR102218457B1 (en) | 2021-02-19 |
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