KR100297425B1 - Surface treatment of aluminum or its alloys - Google Patents
Surface treatment of aluminum or its alloys Download PDFInfo
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- KR100297425B1 KR100297425B1 KR1019980041652A KR19980041652A KR100297425B1 KR 100297425 B1 KR100297425 B1 KR 100297425B1 KR 1019980041652 A KR1019980041652 A KR 1019980041652A KR 19980041652 A KR19980041652 A KR 19980041652A KR 100297425 B1 KR100297425 B1 KR 100297425B1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
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Abstract
본 발명은 알루미늄 또는 그 합금재 피처리물을 탈지(脫脂)후에 포타슘 페라이트가 1∼30g/ℓ의 농도로 함유된 수산화나트륨 용액으로 코팅반응시키는 것을 특징으로 하는 알루미늄 또는 알루미늄-함유 금속의 표면처리방법에 관한 것으로, 알루미늄 또는 그 합금재 피처리물의 표면에 종래의 방법에 의한 것 보다 내식성 및 내박리성이 우수한 코팅층을 형성시킬 수 있고, 또한 표면처리에서 나오는 폐수가 환경친화적이고 그 처리도 종래에 비해 대폭 감소된 비용으로 간단하게 수행할 수 있는 등의 효과가 있다.The present invention provides a surface treatment of an aluminum or aluminum-containing metal, characterized by coating the aluminum or its alloy material with a sodium hydroxide solution containing potassium ferrite at a concentration of 1 to 30 g / l after degreasing. The present invention relates to a method of forming a coating layer on the surface of an aluminum or its alloy material to be treated with corrosion resistance and peeling resistance superior to that of the conventional method, and the wastewater from the surface treatment is environmentally friendly, and the treatment thereof is also conventional. Compared to this, it can be easily performed at a significantly reduced cost.
Description
본 발명은 알루미늄 또는 그 합금의 표면처리방법에 관한 것으로서, 보다 구체적으로는 포타슘 페라이트를 이용한 알루미늄 또는 그 합금의 전처리 코팅방법에 관한 것이다.The present invention relates to a surface treatment method of aluminum or an alloy thereof, and more particularly, to a pretreatment coating method of aluminum or an alloy thereof using potassium ferrite.
알루미늄 또는 그 합금의 표면처리하는 방법으로는 아노다이징(anodizing)이나 크로메이트 컨버젼 코팅(chromate conversion coating) 등이 잘 알려져있다.As a method of surface treatment of aluminum or its alloys, anodizing and chromate conversion coating are well known.
아노다이징은 페인팅시에 적당한 접착력이 있고 봉공처리에 사용되는 첨가제에 의한 색상넣기가 가능하고, 알루미나의 산화깊이가 깊어 부식저항이 매우 우수한 등의 장점이 있으나 전기적 저항이 커서 전기도전재료의 처리가 어려우며, 가격이 고가이고, 처리시간이 매우 길다. 아노다이징은 또한 처리시 전기접촉이 필요하다.Anodizing has the advantages of proper adhesiveness when painting and color filling by additives used in sealing process, and the oxidation depth of alumina is very good, so it has very good corrosion resistance. The price is high and the turnaround time is very long. Anodizing also requires electrical contact during processing.
크로메이트 컨버젼 코팅은 크롬산에 알루미늄 또는 알루미늄-함유 금속을 침지하여 처리하는 처리공정이 단순하며, 크로메이트 컨버젼 코팅 처리후에는 표면에 크롬산 및 알루미늄 산화물층의 복합산화물이 형성되어 이것에 의한 부식저항이 향상되며, 크로메이트 컨버젼 코팅처리된 알루미늄 또는 그 합금은 페인트 성질이 좋고 어느 정도 긁힘에 대한 자기 치유성질이 있다. 또한 크로메이트 컨버젼 코팅처리된 알루미늄 또는 알루미늄-함유 금속은 전자기 부품의 계면부식방지제로서 역할을 겸하게 되며, 동시에 전기전도성이 좋아서 전자기 부품의 가스켓등에 사용된다. 그러나 크로메이트 컨버젼 코팅에 의해 크롬처리된 알루미늄재 부품은 피부와 접촉시 피부염이나 암을 유발하는 것이로 밝혀졌다. 크롬6가의 인체에 대한 피해가 매우 커 작업자의 작업기피 현상이 있고, 선진국에서는 이의 규제방안이 나오고 있는 실정이다. 그러나 크로메이트 컨버젼 코팅처리된 제품의 성능이 매우 우수하기 때문에 많은 곳에서 사용되고 있다.The chromate conversion coating has a simple process of immersing aluminum or aluminum-containing metal in chromic acid, and after the chromate conversion coating, a complex oxide of chromic acid and aluminum oxide layer is formed on the surface, thereby improving corrosion resistance. , Chromate conversion coated aluminum or its alloys have good paint properties and are somewhat self-healing against scratches. In addition, the chromate conversion coated aluminum or aluminum-containing metal serves as an interfacial corrosion inhibitor of the electromagnetic component, and at the same time, it is used for the gasket of the electromagnetic component due to its good electrical conductivity. However, aluminum parts chromed by chromate conversion coatings have been found to cause dermatitis and cancer in contact with the skin. The damage to the human body of chromium 6 is so great that there is a work-avoidance phenomenon of workers, and in advanced countries, the regulations are coming out. However, it is used in many places because the performance of chromate conversion coated products is very good.
상기한 방법 이외에, 크롬산, 인산, 불산 등을 이용하여 알루미늄 또는 그 합금을 표면처리하는 방법들이 알려져 있다. 그러나 이러한 방법들도 작업자의 건강에 악영향을 미친다는 환경보고서들이 등장하게 되어 작업기피현상이 심화되고 있다.In addition to the above-described methods, methods for surface-treating aluminum or alloys thereof using chromic acid, phosphoric acid, hydrofluoric acid, and the like are known. However, the environmental reports that these methods also adversely affect the health of workers have emerged, and work evasion is deepening.
이러한 기술이 발표된 특허문헌의 에를 들면, 크로메이트 처리에 관한 것으로 US 4,451,304호, US 4,191,596호, KS 78-3639, KS 94-28092, KS 95-14931, KS 91-9080 등이 있고, 시안계에 관한 것으로 US 4,036,667, US 4,146,401, US 5,122,202 등이 있으며, 3가 크롬처리에 관한 것으로 US 4,367,099 등이 있다.Examples of patent documents in which such technology has been published include US 4,451,304, US 4,191,596, KS 78-3639, KS 94-28092, KS 95-14931, and KS 91-9080, which relate to chromate treatment. US 4,036,667, US 4,146,401, US 5,122,202, and US Pat. No. 4,367,099.
이러한 기존의 종래 알루미늄 또는 그 합금의 표면처리기술은 대부분이 유독한 크로메이트를 사용함으로 작업자의 안전이 보장되지 않고 또한 제품자체에 잔류하는 크롬이 인체에 해를 미칠수 있으며, 또한 다른 대체기술들에서 사용하고 있는 원소들도 모두 유해한 것들 뿐이어서 폐기물 처리비용이 크고 환경에 악영향을 미치는 등의 문제점을 갖고 있다.This conventional conventional aluminum or its alloy surface treatment technology is mostly used to toxic chromate does not guarantee the safety of the operator and chromium remaining in the product itself may harm the human body, and also in other alternative technologies All of the elements used are also harmful and have problems such as high waste disposal costs and adverse environmental effects.
따라서 본 발명은 상기한 바와 같은 선행기술의 제반 문제점을 감안하여 알루미늄 또는 그 합금을 환경친화적이면서 우수한 코팅성능을 제공하는 새로운 표면처리방법을 제공하는 것을 기술적 과제로 한다.Accordingly, the present invention is to provide a new surface treatment method for providing an environmentally friendly and excellent coating performance of aluminum or its alloy in view of the above problems of the prior art as a technical problem.
도 1은 본 발명의 실시예 2에 의해 알루미늄에 코팅된 코팅층의 전자현미경 사진이고,1 is an electron micrograph of a coating layer coated on aluminum by Example 2 of the present invention,
도 2는 도 1의 코팅층을 WDX로 분석한 결과를 보여주는 그래프이며,Figure 2 is a graph showing the results of analyzing the coating layer of Figure 1 with WDX,
도 3은 도 1의 코팅층을 XPS로 분석한 결과를 보여주는 그래프이고,Figure 3 is a graph showing the results of analyzing the coating layer of Figure 1 by XPS,
도 4는 본 발명의 실시예 5에 의해 알루미늄에 코팅된 코팅층을 WDX로 분석한 결과를 보여주는 그래프이다.Figure 4 is a graph showing the results of the WDX analysis of the coating layer coated on aluminum by Example 5 of the present invention.
상기한 과제를 해결한 본 발명에 의하면, 알루미늄 또는 그 합금재 피처리물을 탈지(脫脂)후에 포타슘 페라이트가 1∼30g/ℓ의 농도로 함유된 수산화나트륨 용액으로 코팅반응시키는 것을 특징으로 하는 알루미늄 또는 그 합금의 표면처리방법이 제공된다.According to the present invention which solves the above-mentioned problems, aluminum or its alloy material is subjected to a coating reaction after degreasing with a sodium hydroxide solution containing potassium ferrite at a concentration of 1 to 30 g / l. Or a surface treatment method of the alloy.
상기한 코팅용액에는 포타슘 페라이트의 코팅을 안정화하기 위한 첨가제로 과망간산 칼륨 1∼10g/ℓ와 Na2S2O80.5-10 g/ℓ를 첨가하거나 또는 NaOCl 5∼10g/ℓ를 첨가하는 것이 바람직하다.It is preferable to add 1-10 g / l of potassium permanganate and 0.5-10 g / l of Na 2 S 2 O 8 or 5-10 g / l of NaOCl to the coating solution as an additive to stabilize the coating of potassium ferrite. Do.
이하, 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
통상의 방법으로 탈지처리한 알루미늄 또는 알루미늄-함유 금속재 피처리물을 본 발명에 따라 포타슘 페라이트가 1∼30g/ℓ의 농도로 함유된 수산화나트륨 용액으로 코팅반응시키면 피처리물의 표면에 황금색 알루미늄과 페라이트계 코팅층이 형성되게 된다. 처리액중 포타슘 페라이트가 1g/ℓ 보다 적은 양으로 함유되면 코팅층이 형성되지 않으며, 30g/ℓ 보다 많은 양으로 함유되면 생성층의 조성이 불균일하게 되고 얼룩이 생길 수가 있으므로 상기한 범위내로 함유시키는 것이 바람직하다.The aluminum or aluminum-containing metal material treated by the conventional method is coated with sodium hydroxide solution containing potassium ferrite at a concentration of 1 to 30 g / l according to the present invention. The coating layer is formed. If potassium ferrite is contained in the treatment solution in an amount less than 1 g / l, the coating layer will not be formed. If it contains more than 30 g / l, the composition of the resulting layer may be uneven and stains may occur. Do.
이 코팅층은 전자현미경으로 촬영한 바 도 1의 사진에 나타나는 바와 같이 코팅층이 치밀함을 알수 있으며, WDX로 분석한 결과 상당량의 Fe가 첨가되어 있음을 알수 있었고(도 2 참조), XPS로 분석한 결과 코팅층이 (FeO)Al2O3와 Fe2O3(Al2O3) 조성의 복합 산화물인 것임을 확인하였다. 이러한 코팅층은 대략 0.5μ 정도의 균일한 두께를 가지며, 기존의 알루미늄의 표면처리 혹은 코팅처리에 비해 내식성 및 내박리성이 우수하여 특히 페인트의 하지 코팅으로 매우 유용하다.The coating layer was taken by electron microscope, and as shown in the photograph of FIG. 1, the coating layer was dense. As a result of analysis with WDX, a considerable amount of Fe was added (see FIG. 2), and analyzed by XPS. As a result, it was confirmed that the coating layer was a complex oxide having a composition of (FeO) Al 2 O 3 and Fe 2 O 3 (Al 2 O 3 ). Such a coating layer has a uniform thickness of about 0.5μ, and excellent in corrosion resistance and peeling resistance compared to the surface treatment or coating treatment of the conventional aluminum is particularly useful as a base coating of paint.
또한 본발명의 표면처리방법은 폐수처리비용이 저렴하다는 특징이 있다. 이는 페라이트 화합물의 폐수처리는 산에 중화만 시켜 바로 처리가 가능하며, 페라이트 화합물이 환경친화적 물질이기 때문이다.In addition, the surface treatment method of the present invention is characterized by low cost of waste water treatment. This is because the wastewater treatment of the ferrite compound can be treated immediately by neutralizing the acid, and the ferrite compound is an environmentally friendly material.
포타슘 페라이트의 제조에 관해서는 잘알려져 있다. 예를 들어 미국특허 4,435,256호에는 전기화학적 방법으로 90% 이상의 순도를 갖는 K2FeO4를 제조하는 것이 설명되어 있다.The production of potassium ferrite is well known. For example, US Pat. No. 4,435,256 describes the preparation of K 2 FeO 4 having a purity of at least 90% by electrochemical methods.
포타슘 페라이트는 증류수에 넣어도 분해되지 않으나 알칼리에서 반응성이 강한 성분으로 수산화나트륨 용액에 일정양을 녹여서 사용한다.Potassium ferrite does not decompose in distilled water, but it is a highly reactive component in alkali and is used by dissolving a certain amount in sodium hydroxide solution.
위에 설명한 바와 같은 본 발명의 특징 및 기타의 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 하기 실시예에서 수행된 내식성과 밀착성은 ASTM B117과 KS D8334-1990법으로 측정하였다.Features and other advantages of the present invention as described above will become more apparent from the embodiments described below. Corrosion resistance and adhesion performed in the following examples were measured by ASTM B117 and KS D8334-1990 method.
내식성: 10초 또는 20초 코팅한 시험편에 ASTM B117에 의거 5% NaCl 수용액을 35℃의 온도에서 110 내지 200시간 분무하여 수행. 1-10 등급으로 나누고 높은 등급일 수록 내식성이 우수함.Corrosion resistance: 10 seconds or 20 seconds coated test piece by spraying 5% NaCl aqueous solution according to ASTM B117 at a temperature of 35 ℃ 110 to 200 hours. Divided into 1-10 grades, the higher the grade, the better the corrosion resistance.
밀착성: 코팅시험편에 칼로 모눈을 새기고 테이프를 붙였다 떼어 코팅이 박리되는 정도를 시험.Adhesiveness: Test the degree of coating peeling by carving a grid with a knife on a coating test piece and then peeling it off.
또한, 알루미늄 시편은 코팅처리하기 전에 탈지처리는 알칼리 세척에 의한 표면 세척 및 수세 후 0.1% 질산용액에서 산세처리 후 수세처리하는 것으로 수행하였다.In addition, the aluminum specimen was subjected to degreasing treatment before the coating treatment, surface washing by alkali washing and washing with water after pickling in 0.1% nitric acid solution after washing with water.
[실시예 1]Example 1
0.1 M의 수산화나트륨 수용액에 NaOCl 10g/ℓ 및 하기 표에 제시되는 바와 같은 양의 포타슘 페라이트(K2FeO4)를 넣어 코팅용액을 제조하였다. 제조된 코팅용액에 탈지처리된 1,000 계열 및 6,000 계열 알루미늄을 각각 침지하여 코팅처리한 후 수세하고 자연건조하였다. 그 후 밀착력 향상을 위하여 100℃의 증류수에서 열처리하였다. 결과의 시편에 대해서 내식성 및 밀착성을 측정하였다. 그 결과는 하기 표 1에 제시된다.NaOCl 10g / L and potassium ferrite (K 2 FeO 4 ) of the amount as shown in the following table in 0.1 M aqueous sodium hydroxide solution to prepare a coating solution. The coated solution was immersed in 1,000 series and 6,000 series aluminum degreased, and then washed with water and naturally dried. Thereafter, heat treatment was performed in distilled water at 100 ° C. to improve adhesion. Corrosion resistance and adhesion were measured for the resulting specimens. The results are shown in Table 1 below.
또한 얻어진 시편에 대해서 코팅층을 WDX에 의해 분석한 결과 코팅층에 상당량의 Fe가 첨가되어 있음을 알 수 있었고(도2 참조), 이를 XPS로 정밀분석한 결과 코팅층이 (FeO)Al2O3, Fe2O3(Al2O3) 조성의 복합산화물임을 알수 있었다(도3참조).Also was found that a considerable amount of Fe is added to the resulting coating layer was analyzed by a coating layer on the WDX For the obtained specimens (see Fig. 2), the resulting coating layer by fine analyzed by XPS (FeO) Al 2 O 3, Fe 2 O 3 (Al 2 O 3 ) was found to be a composite oxide composition (see Fig. 3).
[실시예 5]Example 5
1 M의 NaOH 수용액에 KMnO410 g/ℓ, Na2S2O85 g/ℓ, K2FeO410 g/ℓ를 넣어 제조한 코팅용액을 사용하고 시편으로 탈지처리한 6,000계 알루미늄을 사용한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다. 결과의 시편에 대해서 코팅층을 WDX에 의해 분석한 결과 코팅층에 상당량의 Fe가 첨가되어 있음을 알 수 있었다(도4 참조).Using a coating solution prepared by adding 10 g / l of KMnO 4, 5 g / l of Na 2 S 2 O 8 and 10 g / l of K 2 FeO 4 to a 1 M aqueous NaOH solution, 6,000 series aluminum degreased with a specimen was used. The same procedure as in Example 1 was repeated except that it was used. As a result of analyzing the coating layer by WDX on the resulting specimen, it was found that a considerable amount of Fe was added to the coating layer (see FIG. 4).
위에 설명한 바와 같이 본발명은 알루미늄 또는 그 합금재 피처리물의 표면에 종래의 방법에 의한 것 보다 내식성 및 내박리성이 우수한 코팅층을 형성시킬 수 있고, 또한 표면처리에서 나오는 폐수가 환경친화적이고 그 처리도 종래에 비해 대폭 감소된 비용으로 간단하게 수행할 수 있는 등의 효과가 있다.As described above, the present invention can form a coating layer having excellent corrosion resistance and peeling resistance on the surface of an aluminum or its alloy material to be treated by conventional methods, and wastewater from the surface treatment is environmentally friendly and its treatment. In addition, there is an effect that can be easily performed at a significantly reduced cost compared to the prior art.
Claims (3)
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| KR1019980041652A KR100297425B1 (en) | 1998-10-02 | 1998-10-02 | Surface treatment of aluminum or its alloys |
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| KR1019980041652A KR100297425B1 (en) | 1998-10-02 | 1998-10-02 | Surface treatment of aluminum or its alloys |
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