KR101074165B1 - Zn-Ni alloy electrodeposition composition - Google Patents
Zn-Ni alloy electrodeposition composition Download PDFInfo
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- KR101074165B1 KR101074165B1 KR1020090003093A KR20090003093A KR101074165B1 KR 101074165 B1 KR101074165 B1 KR 101074165B1 KR 1020090003093 A KR1020090003093 A KR 1020090003093A KR 20090003093 A KR20090003093 A KR 20090003093A KR 101074165 B1 KR101074165 B1 KR 101074165B1
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Abstract
본 발명은 아연-니켈 합금전착용 조성물에 관한 것으로 아연-니켈 기본 조성액에 니켈과 아연의 전착특성을 향상시키는 착화제(Sodium citrate, 80~120 ml/K.A.H), 고밀도와 광택을 내게 하는 광택제(술폰산계, 180~220 ml/K.A.H) 및 니켈이온이 침전됨을 방지하는 첨가제(2,2',2"-nitrilotriethanol, Nickel Sulfate 2종, 40g/l)가 함유된 아연-니켈 합금 전기 도금용 조성물이다.The present invention relates to a zinc-nickel alloy electrodeposition composition, a complexing agent (Sodium citrate, 80-120 ml / KAH) to improve the electrodeposition properties of nickel and zinc in the zinc-nickel base composition liquid, a high-density and glossy polish ( Zinc-nickel alloy electroplating composition containing sulfonic acid, 180 ~ 220 ml / KAH) and additives (2,2 ', 2 "-nitrilotriethanol, 2 kinds of Nickel Sulfate, 40g / l) to prevent precipitation of nickel ions to be.
상기 본 발명의 아연-니켈 합금전착용 조성물은 무시안 알칼리 아연 합금 도금용액으로써 실험실적으로 합성한 여러 가지 첨가제들로 조성된 친환경 도금용액이며, 사용시 도금층의 니켈공석율을 현저히 향상시키고 기존의 아연도금에 비해 나노상(nano-phase)이며, 내식 및 경도가 매우 우수하고 특히, 무결점(blister free), 연성(ductile), 균일한 코팅성(easy-to-passivate coatings)이 탁월하다. The zinc-nickel alloy electrodeposition composition of the present invention is an environmentally friendly plating solution composed of various additives synthesized by laboratory as an alkali zinc alloy plating solution, and significantly improves the nickel vacancy rate of the plating layer and uses the existing zinc. It is nano-phase compared to plating, has excellent corrosion resistance and hardness, and is particularly excellent in blister free, ductile, and easy-to-passivate coatings.
아연, 니켈, 합금, 전착, 조성물, 착화제, 광택제, 니켈공석율, 나노 Zinc, nickel, alloy, electrodeposition, composition, complexing agent, brightener, nickel vacancy rate, nano
Description
본 발명은 아연-니켈 합금전착용 조성물에 관한 것으로 아연-니켈 기본 조성액에 니켈과 아연의 전착특성을 향상시키는 착화제, 고밀도와 광택을 내게 하는 광택제 및 니켈이온이 침전됨을 방지하는 첨가제가 함유된 아연-니켈 합금 전기 도금용 조성물이다.The present invention relates to a zinc-nickel alloy electrodeposition composition comprising a complexing agent that improves the electrodeposition properties of nickel and zinc in a zinc-nickel base composition solution, a high density and gloss brightening agent, and an additive that prevents precipitation of nickel ions. Zinc-nickel alloy electroplating composition.
상기 본 발명의 아연-니켈 합금전착용 조성물은 무시안 알칼리 아연 합금 도금용액으로써 실험실적으로 합성한 여러 가지 첨가제들로 조성된 친환경 도금용액이며, 사용시 도금층의 니켈공석율을 현저히 향상시키고 기존의 아연도금에 비해 나노상(nano-phase)이며, 내식 및 경도가 매우 우수하고 특히, 무결점(blister free), 연성(ductile), 균일한 코팅성(easy-to-passivate coatings)이 탁월하다. The zinc-nickel alloy electrodeposition composition of the present invention is an environmentally friendly plating solution composed of various additives synthesized by laboratory as an alkali zinc alloy plating solution, and significantly improves the nickel vacancy rate of the plating layer and uses the existing zinc. It is nano-phase compared to plating, has excellent corrosion resistance and hardness, and is particularly excellent in blister free, ductile, and easy-to-passivate coatings.
종래 빌딩이나 구조물 구축용, 주택, 자동차 본체 등에 아연도금이나 용융아연합금도금 등의 방법이 많이 사용되고 있다.Conventionally, methods such as zinc plating and hot dip zinc alloy plating have been used for buildings, structures, houses, automobile bodies, and the like.
특히 용융아연합금도금의 경우 내식성 향상을 위하여 사용되는데 이는 아연 이라는 금속이 양호한 활성을 가짐으로써 조직이 치밀한 아연합금 형태를 만듦으로써 내식성이 증가하기 때문이다. Especially in the case of hot-dip zinc alloy plating, it is used to improve the corrosion resistance because the metal of zinc has a good activity and thus the corrosion resistance is increased by forming a dense zinc alloy structure.
아연의 부식율은 부식된 금속체의 성질과 형태 그리고 주위의 부식 환경에 크게 좌우된다. 예를 들면 유황성분을 함유한 가스, 산 또는 알칼리성분이 가득 찬 주위 환경 하에서는 내식성이 좋다는 아연합금이라도 각각 유화물 산화물 또는 알칼리와 반응한 용체(solution)가 되어 부식이 빨라지게 마련이다. 따라서 철판에 아연층을 피복(도금)시킨 것을 부식되지 않도록 하게 하려면 상술한 부식환경속에서 벗어나도록 해야 한다. 그런데 아연이 중성(中性) 분위기하에서 도금될 때에는 그 산물인 아연합금은 치밀한 조직이 되고 중성용액에서의 용해(부식)가 불가능하게 할 수가 있으므로 중성분위기하에서 염화이온(chlorine ion) 농도를 제어하는 등의 기술이 선보이고 있다. The corrosion rate of zinc is highly dependent on the nature and form of the corroded metal body and the surrounding corrosion environment. For example, in an ambient environment filled with sulfur, gas, acid, or alkali components, even zinc alloys having good corrosion resistance become solutions that react with sulfide oxides or alkalis, respectively, to accelerate corrosion. Therefore, in order to prevent corrosion of the coating (plating) of the zinc layer on the iron plate, it must be released from the above-mentioned corrosion environment. However, when zinc is plated in a neutral atmosphere, the product zinc alloy becomes a dense structure and may not be able to dissolve (corrosive) in a neutral solution, thereby controlling the concentration of chlorine ion in a medium atmosphere. And other technologies are being introduced.
최근에는 내식성이나 경도, 흑색도 등의 향상을 위해 니켈성분이 추가된 아연-니켈 합금도금이 소개되고 있다.Recently, zinc-nickel alloy plating with an added nickel component has been introduced to improve corrosion resistance, hardness, and blackness.
일반적으로, 아연-니켈 합금도금 강판은 도금층의 니켈 함량에 따라 내식성을 비롯한 프레스 성형성, 용접성, 도장성 등 각종 품질 특성이 영향을 받게 되며, 제반특성 측면에서 적정 니켈 함량은 10-15wt% 범위인 것으로 알려져 있다. 그러나, 자동차용 강판으로 성형성, 용접성 등의 향상을 위해서는 도금층의 니켈 함량을 12wt%이상으로 높이는 것이 유리하며, 실제 강판 제조업체에서도 도금층의 니켈 함량을 높여서 공급하는 실정이다.In general, zinc-nickel alloy plated steel sheet is affected by various quality characteristics such as corrosion resistance, press formability, weldability, paintability, etc., depending on the nickel content of the plating layer, the appropriate nickel content in the range of 10-15wt%. It is known to be. However, it is advantageous to increase the nickel content of the plated layer to more than 12wt% in order to improve the formability, weldability, etc. as a steel sheet for automobiles, and the actual steel sheet manufacturers also increase the nickel content of the plated layer.
아연-니켈 합금도금은 일반적으로 염화물계 혹은 황산염계 도금액에서 실시 되는데 비(卑)한 금속(전위가 낮은 금속)인 아연이 귀한 금속인 니켈보다 우선적으로 석출하는 이상형 공석 현상을 나타내어 니켈 석출비가 낮아지게 된다. Zinc-nickel alloy plating is generally carried out in chloride or sulfate plating solution, and zinc, which is a non-metal (low-potential metal), exhibits an ideal vacancy phenomenon that preferentially precipitates over nickel, which is a precious metal. You lose.
염화물계 도금액은 황산염계에 비해 이상형 공석 정도는 적지만 도금층의 니켈 함량은 도금액의 니켈이온 농도보다 낮아지게 된다. 특히, 가용성 양극을 사용하는 염화물계 도금액의 경우 니켈 석출비가 낮게 되면 도금시간이 경과함에 따라 도금액의 니켈 농도는 점점 증가하게 되어 도금액의 안정된 관리를 어렵게 한다.Chloride-based plating solution is less than the vacancy-based ideal vacancy, but the nickel content of the plating layer is lower than the nickel ion concentration of the plating solution. In particular, in the case of a chloride plating solution using a soluble anode, if the nickel deposition ratio is low, the nickel concentration of the plating solution gradually increases as the plating time elapses, making it difficult to stably manage the plating solution.
염화물계 도금액에서 도금층의 니켈 함량을 증가시키기 위하여 도금액의 온도나 니켈이온의 농도, 염화칼륨, 염화나트륨, 염화암모늄 등의 지지전해질 농도를 증가시키는 방법 등이 제안되어 있으나 도금액이 불안정하게 되고 표면품질도 열화되는 문제점이 있다. 특히 표면품질 향상을 위하여 상용 첨가제를 사용하는 경우 통상 도금층의 니켈 함량을 더욱 감소시키게 되며, 도금층의 니켈 함량 조정을 어렵게 하는 요인이 된다.In order to increase the nickel content of the plating layer in the chloride plating solution, a method of increasing the temperature of the plating solution, the concentration of nickel ions, the support electrolyte concentration of potassium chloride, sodium chloride, ammonium chloride, etc. has been proposed, but the plating solution becomes unstable and the surface quality deteriorates. There is a problem. In particular, when a commercial additive is used to improve the surface quality, the nickel content of the plating layer is further reduced, which is a factor that makes it difficult to adjust the nickel content of the plating layer.
이런 문제를 개선하기 위해 특히 자동차용 강판으로 많이 사용되는 아연-니켈 합금전기도금 강판을 제조하는데 있어서 고전류밀도 조건에서 합금도금층의 니켈 함량을 높일 수 있는 아연-니켈 전기도금액 제조방법으로서 염화물계 도금액에 유기물 혹은 금속 이온을 소량 첨가하여 니켈공석율을 높이는 기술이 소개되고 있으나 염화물계의 기본적인 특성으로 인해 여전히 니켈함량이 충분하지 못하여 내식성과 내열성이 불충분하다.In order to improve this problem, especially in the manufacture of zinc-nickel alloy electroplating steel sheet which is widely used as automotive steel sheet, it is a chloride-based plating solution as a method of manufacturing zinc-nickel electroplating liquid which can increase the nickel content of the alloy plating layer under high current density conditions. The technique of increasing the nickel vacancy rate by adding a small amount of organic or metal ions to the metal is introduced, but due to the basic characteristics of the chloride system, the nickel content is still insufficient and thus the corrosion resistance and heat resistance are insufficient.
이에 본 발명은 종래 기술의 문제점을 해결하기 위한 것으로, 아연-니켈 기본 조성액에 착화제 등의 소정 성분을 첨가함으로써 도금층의 니켈공석율을 현저히 향상시켜 내식성과 내열성을 향상시킬 수 있는 아연-니켈 합금전착용 조성물을 제공하고자 한다.Accordingly, the present invention is to solve the problems of the prior art, zinc-nickel alloy that can significantly improve the nickel vacancy rate of the plating layer by adding a predetermined component such as a complexing agent to the zinc-nickel base composition liquid to improve the corrosion resistance and heat resistance To provide a composition for electrodeposition.
본 발명은 아연-니켈 기본 조성액에 니켈과 아연의 전착특성을 향상시키는 착화제, 고밀도와 광택을 내게 하는 광택제 및 니켈이온이 침전됨을 방지하는 첨가제가 함유된 것이 특징이다.The present invention is characterized in that the zinc-nickel base composition contains a complexing agent that improves the electrodeposition properties of nickel and zinc, a brightening agent that gives high density and gloss, and an additive that prevents precipitation of nickel ions.
상기 본 발명의 아연-니켈 합금전착용 조성물은 무시안 알칼리 아연 합금 도금용액으로써 실험실적으로 합성한 여러 가지 첨가제들로 조성된 친환경 도금용액이며, 사용시 도금층의 니켈공석율을 현저히 향상시키고 기존의 아연도금에 비해 나노상이며, 내식 및 경도가 매우 우수하고 특히, 무결점, 연성, 균일한 코팅성이 탁월하다. The zinc-nickel alloy electrodeposition composition of the present invention is an environmentally friendly plating solution composed of various additives synthesized by laboratory as an alkali zinc alloy plating solution, and significantly improves the nickel vacancy rate of the plating layer and uses the existing zinc. It is nanophase compared with plating, and is very excellent in corrosion resistance and hardness, and is particularly excellent in defect free, softness, and uniform coating.
상기 목적을 달성하기 위하여, 본 발명은 아연-니켈 기본 조성액에 니켈과 아연의 전착특성을 향상시키는 착화제, 고밀도와 광택을 내게 하는 광택제 및 니켈이온이 침전됨을 방지하는 첨가제가 함유된 아연-니켈 합금 전기 도금용 조성물이 특징이다.In order to achieve the above object, the present invention is zinc-nickel containing a complexing agent to improve the electrodeposition properties of nickel and zinc, a high-density and glossing agent and an additive to prevent the precipitation of nickel ions in the zinc-nickel base composition It features a composition for alloy electroplating.
여기서, 상기 아연-니켈 기본 조성액은 ZnO 3~10vol%, NaOH 81~94vol% 및 NiSO46H2O 3~9vol%로 이루어진다.Here, the zinc-nickel base composition is composed of ZnO 3 ~ 10vol%, NaOH 81 ~ 94vol% and NiSO 4 6H 2 O 3 ~ 9vol%.
또한, 상기 착화제로는 구연산나트륨 80~120 ml/K.A.H, 고밀도와 광택을 내게 하는 광택제로는 술폰산계 광택제 180~220 ml/K.A.H 그리고 니켈이온이 침전됨을 방지하는 첨가제로는 2,2',2"-니트로트리에탄올과 황산니켈 혼합액 30~50g/l가 바람직하다.In addition, the complexing agent is sodium citrate 80 ~ 120 ml / KAH, the high density and the gloss to give a gloss sulfonic acid-based polish agent 180 ~ 220 ml / KAH and as an additive to prevent the precipitation of nickel ions 2,2 ', 2 30-50 g / l of "-nitrotriethanol and nickel sulfate liquid mixture is preferable.
또한, 기타 첨가제로써 모노에탄올아민, 글루콘산소다, 에틸렌디아민테트라아세트산, 니코틴산, 폴리이민 또는 에틸렌글리콜을 적당량(0.1~0.3 vol%) 첨가할 수 있다.As other additives, an appropriate amount (0.1 to 0.3 vol%) of monoethanolamine, sodium gluconate, ethylenediaminetetraacetic acid, nicotinic acid, polyimine or ethylene glycol can be added.
이하, 실시예를 통하여 좀더 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
실시예Example
일반적인 도금공정인 알카리탈지→전해탈지→산세침적→도금→수세→건조의 공정을 거치되 상기 도금공정에 본 발명의 아연/니켈함금도금 전착용 조성물을 사용하여 샘플을 얻었다.Alkaline degreasing → electrolytic degreasing → pickling deposition → plating → washing → drying, which is a general plating process, was used, but samples were obtained using the zinc / nickel alloy plating electrodeposition composition of the present invention in the plating process.
<조건><Condition>
온도 10~35℃, 시간 10분 Temperature 10-35 degrees Celsius, time ten minutes
음극전류밀도 0.5~4.5(A/dm2)Cathode Current Density 0.5 ~ 4.5 (A / dm 2 )
양극전류밀도 2~3(A/dm2)Anode Current Density 2 ~ 3 (A / dm 2 )
양극판으로서 철판에 니켈도금 또는 니켈판 사용 Nickel plated or nickel plated on iron plate as positive plate
여과 및 교반은 하지 않음No filtration and stirring
<아연/니켈함금도금에 사용되는 전착용 조성물>Electrodeposition Composition for Zinc / Nickel Plating
아연-니켈 기본 조성액으로서 ZnO 10g/l, NaOH 120g/l 및 NiSO46H2O 8g/l 의 기본 조성액에 착화제로서 구연산나트륨(Sodium citrate) 80g ml/K.A.H, 술폰산계광택제 180 ml/K.A.H 및 첨가제로서 2,2',2"-니트로트리에탄올과 황산니켈(Nickel Sulfate) 혼합액 40g/l으로 구성된 아연-니켈 합금전착용 조성물ZnO 10g / l, NaOH 120g / l and NiSO 4 6H 2 O 8g / l as the zinc-nickel base liquid solution, sodium citrate 80g ml / KAH as a complexing agent, 180 ml / KAH sulfonic acid-based varnish, and Zinc-nickel alloy electrodeposition composition consisting of 40 g / l of 2,2 ', 2 "-nitrotriethanol and nickel sulfate mixture as an additive
상기 본 발명의 실시예에서 얻어진 샘플과 현재 시판중인 국내,외 샘플(비교예 1,2)에 대한 SEM, XRF, XRD 분석 결과를 도면과 표에서 확인할 수 있다.SEM, XRF, and XRD analysis of the samples obtained in Examples of the present invention and domestic and foreign samples (comparative examples 1 and 2) currently on the market can be confirmed in the drawings and the tables.
도 1a~c는 각 샘플들에 대하여 10,000배 확대한 SEM 사진으로서 각 샘플들은 입자의 사이즈가 대동소이하고 도 1a(비교예 1), 도 1b(비교예 2)에 비해 실시예의 경우(도 1c)가 훨씬 결정립 크기가 작음을 확인할 수 있었다. Figures 1a to c is a SEM image of 10,000 times magnification for each sample, each sample is of the same size of the particles and compared to Figure 1a (Comparative Example 1), Figure 1b (Comparative Example 2) in the case of the embodiment (Fig. 1c ) Showed much smaller grain size.
도 2는 도 1c를 다시 30,000배 확대한 SEM 사진이다. 상기 도 1a,b에서 확인되는 비교예의 아연-니켈 합금의 grain size는 0.1~0.4마이크로정도(100~400nm)이나 30,000배 확대한 도 2의 본 실시예는 20~50nm정도로 미세한 알갱이들이 코팅되어 있음을 알 수 있었다.FIG. 2 is an SEM image of FIG. 1C enlarged again 30,000 times. The grain size of the zinc-nickel alloy of the comparative example confirmed in FIGS. 1a and b is about 0.1 to 0.4 microns (100 to 400 nm), but this example of FIG. 2 magnified 30,000 times is coated with fine grains of about 20 to 50 nm. And it was found.
각 샘플들에 대한 XRD 분석 결과를 도 3a~c에서 확인할 수 있다.XRD analysis results for each sample can be found in FIGS. 3A-C.
도면에서 각 샘플들은 고전류에서 저전류까지 큰 차이 없이 동일한 XRD패턴을 보였다. 전형적인 감마상의 아연니켈 합금 XRD패턴인 Ni3Zn22(411, 330) (642)을 확인할 수 있었다. In the figure, each sample showed the same XRD pattern without a large difference from high current to low current. Ni 3 Zn 22 (411, 330) (642), which is a typical gamma zinc nickel alloy XRD pattern, was identified.
또한, 각 샘플들의 XRF 분석결과, 하기 표 1에서와 같이 비교예 1,2의 경우 니켈의 함량이 15~18%를 보였으나 본 발명의 실시예의 샘플은 비교예 보다도 니켈함량이 평균 5%이상 높은 것을 확인하였다.In addition, as a result of XRF analysis of each sample, as shown in Table 1, in the case of Comparative Examples 1 and 2 showed a nickel content of 15 to 18%, but in the sample of the present invention, the average nickel content of the sample of more than 5% than the comparative example It confirmed that it was high.
이와 같이 니켈함량이 높아지면 내식성과 내열성이 좋아지고 이후 3가 크로메이트 코팅 이후 테스트를 하면 기존 아연도금에 있어서의 3가 크로메이트 보다 십수배의 내식성 향상이 예상된다.As the nickel content increases, the corrosion resistance and heat resistance are improved, and after the trivalent chromate coating test, the corrosion resistance is expected to be improved tens of times than that of the conventional trivalent chromate.
도 1a~c는 각 샘플들에 대하여 10,000배 확대한 SEM 사진Figures 1a-c is a SEM photograph of 10,000 times magnification for each sample
도 2는 도 1c를 다시 30,000배 확대한 SEM 사진FIG. 2 is an SEM image of FIG. 1C enlarged again 30,000 times.
도 3a~c는 각 샘플들에 대한 XRD 분석 결과 그래프Figure 3a ~ c is a graph of the XRD analysis results for each sample
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