KR20220040912A - Method for removing the anodic oxide film on the aluminum surface - Google Patents
Method for removing the anodic oxide film on the aluminum surface Download PDFInfo
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- KR20220040912A KR20220040912A KR1020200124208A KR20200124208A KR20220040912A KR 20220040912 A KR20220040912 A KR 20220040912A KR 1020200124208 A KR1020200124208 A KR 1020200124208A KR 20200124208 A KR20200124208 A KR 20200124208A KR 20220040912 A KR20220040912 A KR 20220040912A
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
- C23G1/125—Light metals aluminium
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
Abstract
Description
본 발명은 알루미늄 표면에 형성된 양극산화막의 제거방법에 관한 것으로, 더욱 상세하게는 알루미늄의 표면에 형성된 양극산화막의 제거효율이 우수할 뿐만 아니라, 알루미늄의 부식을 억제할 수 있는 알루미늄 표면에 형성된 양극산화막의 제거방법에 관한 것이다.The present invention relates to a method for removing an anodized film formed on the surface of aluminum, and more particularly, an anodized film formed on the surface of aluminum that has excellent removal efficiency of the anodized film formed on the surface of aluminum and can suppress corrosion of aluminum. It relates to a method of removal.
알루미늄 양극산화(anodizing)는 알루미늄 표면에 산화알루미늄과 같은 피막을 형성하는 것으로, 알루미늄을 전해액 내에서 양극(anode)으로 하고 통전(通電)시켜 알루미늄의 표면을 산화시키는 방법이다.Aluminum anodizing is a method of oxidizing the surface of aluminum by forming a film such as aluminum oxide on the surface of aluminum.
상기의 과정을 통해 양극산화된 알루미늄은 예컨대, TFT-LCD 제조 장비, 반도체 제조 장비 등의 전극, 디퓨져(diffuser)와 같은 산업용 소재로서 다양하게 이용된다.Aluminum anodized through the above process is variously used as an industrial material such as, for example, an electrode of TFT-LCD manufacturing equipment, semiconductor manufacturing equipment, etc., and a diffuser.
상기 산업용 소재로서 사용되는 양극 산화된 알루미늄은 예컨대, 플라즈마, 고온의 열, 불소 가스, 염소 가스와 같은 가혹한 환경에 노출되기 때문에, 오랜 기간 계속 사용하면 모재 표면의 산화알루미늄 피막에 크랙과 부식이 발생될 수 있기 때문에, 양극산화 알루미늄을 일정 시간 동안 사용한 후에 산화 알루미늄 피막을 재생하는 작업을 진행하게 된다.Anodized aluminum used as the industrial material is exposed to harsh environments such as plasma, high temperature heat, fluorine gas, and chlorine gas. Because it can be, the work of regenerating the aluminum oxide film is carried out after using the anodized aluminum for a certain period of time.
종래에는 산화알루미늄 피막을 재생하기 위해 표면이 오염되고 크랙이 발생한 양극산화 알루미늄을 높은 농도(질량농도가 약 80 wt%)의 수산화나트륨 용액에 침지하여 알루미늄 모재로부터 산화알루미늄 피막을 제거하고, 상기 알루미늄 모재를 다시 양극산화하는 과정을 진행하였다.Conventionally, in order to regenerate the aluminum oxide film, the aluminum oxide film is removed from the aluminum base material by immersing anodized aluminum with a cracked surface in a high concentration (mass concentration of about 80 wt%) sodium hydroxide solution, and the aluminum The process of anodizing the base material again was carried out.
그러나, 상기와 같이 강한 알칼리성의 수산화나트륨(NaOH) 용액으로 인해 산화알루미늄 피막뿐만 아니라 알루미늄 모재도 부식되는 현상이 발생하여 제품의 두께가 점차적으로 얇아지게 되어 기계적 물성이 저하되며, 상기와 같은 재생작업을 수 차례 반복하게 되면 알루미늄 제품에 형성된 홀의 크기가 처음에 설계된 치수를 벗어나게 되어 폐기해야하는 문제점이 있었다.However, due to the strong alkaline sodium hydroxide (NaOH) solution as described above, not only the aluminum oxide film but also the aluminum base material is corroded, and the thickness of the product gradually becomes thinner, and the mechanical properties are reduced, and the regeneration operation as described above If the process is repeated several times, the size of the hole formed in the aluminum product deviated from the initially designed dimension, and there was a problem that it had to be discarded.
본 발명의 목적은 알루미늄의 표면에 형성된 양극산화막의 제거효율이 우수할 뿐만 아니라, 알루미늄의 부식을 억제할 수 있는 알루미늄 표면에 형성된 양극산화막의 제거방법을 제공하는 것이다.It is an object of the present invention to provide a method for removing an anodized film formed on the surface of aluminum that is excellent in removal efficiency of the anodized film formed on the surface of aluminum and can suppress corrosion of aluminum.
본 발명의 목적은 양극산화막이 형성된 알루미늄을 표면에 불순물을 제거하는 불순물제거단계, 상기 불순물제거단계를 통해 불순물이 제거된 알루미늄을 산성분에 침지하여 양극산화막을 제거하는 산성분침지단계 및 상기 산성분침지단계를 통해 양극산화막이 제거된 알루미늄의 표면을 알칼리수로 세척하는 알칼리수세척단계로 이루어지는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법을 제공함에 의해 달성된다.An object of the present invention is an impurity removal step of removing impurities from the surface of aluminum having an anodized film formed thereon, an acidic powder immersion step of immersing the aluminum from which impurities have been removed through the impurity removal step in an acidic component to remove the anodized film, and the acid It is achieved by providing a method for removing the anodization film formed on the aluminum surface, characterized in that it consists of an alkaline water washing step of washing the surface of the aluminum from which the anodization film has been removed through the minute immersion step with alkaline water.
본 발명의 바람직한 특징에 따르면, 상기 불순물제거단계는 양극산화막이 형성된 알루미늄의 표면을 철사모로 연마하여 이루어지는 것으로 한다.According to a preferred feature of the present invention, the step of removing impurities is made by grinding the surface of the aluminum on which the anodized film is formed with a wire bristles.
본 발명의 더 바람직한 특징에 따르면, 상기 철사모는 100 내지 300㎏f/mm2의 강도를 나타내며 0.1 내지 0.5mm의 직경으로 형성되는 것으로 한다.According to a more preferred feature of the present invention, the wire hair represents a strength of 100 to 300 kgf/mm 2 and is to be formed with a diameter of 0.1 to 0.5 mm.
본 발명의 더욱 바람직한 특징에 따르면, 상기 산성분침지단계는 4 내지 5시간 동안 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the acidic minute immersion step is performed for 4 to 5 hours.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 산성분은 pH가 1.5 내지 5.5이며, 질산, 인산, 황산, 염산, 주석산, 및 옥살산으로 이루어진 그룹에서 선택된 하나 이상이 함유되는 것으로 한다.According to an even more preferred feature of the present invention, the acid component has a pH of 1.5 to 5.5, and contains at least one selected from the group consisting of nitric acid, phosphoric acid, sulfuric acid, hydrochloric acid, tartaric acid, and oxalic acid.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 불순물제거단계와 상기 산성분침지단계 사이에는 상기 불순물제거단계를 통해 불순물이 제거된 알루미늄을 산화막 환원제에 침지하는 산화막환원단계가 더 진행되는 것으로 한다.According to a further preferred feature of the present invention, an oxide film reduction step of immersing the aluminum from which impurities have been removed through the impurity removing step in an oxide film reducing agent is further performed between the impurity removal step and the acidic powder immersion step.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 산화막 환원제는 히드라진계 화합물 또는 차인산계 화합물이 0.2 내지 20 중량% 함유되는 것으로 한다.According to an even more preferred feature of the present invention, the oxide film reducing agent is to contain 0.2 to 20% by weight of a hydrazine-based compound or a hypophosphorous acid-based compound.
본 발명에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법은 알루미늄의 표면에 형성된 양극산화막의 제거효율이 우수할 뿐만 아니라, 알루미늄의 부식을 억제할 수 있는 탁월한 효과를 나타낸다.The method for removing the anodic oxide film formed on the surface of aluminum according to the present invention exhibits an excellent effect of suppressing corrosion of aluminum as well as having excellent removal efficiency of the anodization film formed on the surface of aluminum.
도 1은 본 발명의 일 실시예에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법을 나타낸 순서도이다.
도 2는 본 발명의 다른 실시예에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법을 나타낸 순서도이다.
도 3은 본 발명의 실시예 1 내지 2 및 비교예 1 내지 3을 통해 양극산화막이 제거된 알루미늄의 단면을 주사전자현미경(SEM)으로 촬영하여 나타낸 사진이다.
도 4는 본 발명의 실시예 1 내지 2 및 비교예 1 내지 3의 과정을 거치면서 알루미늄의 무게 변화를 측정하여 나타낸 그래프이다.1 is a flowchart illustrating a method for removing an anodization film formed on an aluminum surface according to an embodiment of the present invention.
2 is a flowchart illustrating a method for removing an anodization film formed on an aluminum surface according to another embodiment of the present invention.
3 is a photograph showing a cross-section of aluminum from which an anodization film has been removed in Examples 1 to 2 and Comparative Examples 1 to 3 of the present invention by using a scanning electron microscope (SEM).
4 is a graph showing the change in weight of aluminum through the processes of Examples 1 to 2 and Comparative Examples 1 to 3 of the present invention.
이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.Hereinafter, a preferred embodiment of the present invention and the physical properties of each component will be described in detail, which is intended to describe in detail enough that a person of ordinary skill in the art to which the present invention pertains can easily carry out the invention, This does not mean that the technical spirit and scope of the present invention is limited.
본 발명에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법은 양극산화막이 형성된 알루미늄을 표면에 불순물을 제거하는 불순물제거단계(S101), 상기 불순물제거단계(S101)를 통해 불순물이 제거된 알루미늄을 산성분에 침지하여 양극산화막을 제거하는 산성분침지단계(S103) 및 상기 산성분침지단계(S103)를 통해 양극산화막이 제거된 알루미늄의 표면을 알칼리수로 세척하는 알칼리수세척단계(S105)로 이루어진다.The method for removing the anodic oxide film formed on the surface of aluminum according to the present invention includes an impurity removal step (S101) of removing impurities from the surface of aluminum on which an anodization film is formed, and aluminum from which impurities have been removed through the impurity removal step (S101) into an acidic component. It consists of an acidic minute immersion step (S103) of immersing in to remove the anodized film, and an alkaline water washing step (S105) of washing the surface of the aluminum from which the anodized film has been removed through the acidic minute immersion step (S103) with alkaline water.
상기 불순물제거단계(S101)는 양극산화막이 형성된 알루미늄을 표면에 불순물을 제거하는 단계로, 상기 양극산화막이 형성된 알루미늄의 표면을 철사모로 연마하여 이루어지는데, 상기와 같이 철사모로 알루미늄의 표면을 연마하게 되면 알루미늄의 표면에 형성된 불순물과 양극산화막의 일부가 물리적으로 제거된다.The impurity removal step (S101) is a step of removing impurities from the surface of the aluminum on which the anodization film is formed. When this is done, the impurities formed on the surface of the aluminum and a part of the anodization film are physically removed.
이때, 상기 불순물제거단계(S101)는 강도가 100 내지 300㎏f/mm2인 철사모를 이용하여 이루어지는데, 상기 철사모는 직경이 0.1 내지 0.5mm인 것을 사용하는 것이 바람직하다.At this time, the impurity removal step (S101) is made using a wire hair having a strength of 100 to 300 kgf/mm 2 , it is preferable to use a wire hair having a diameter of 0.1 to 0.5 mm.
더욱 상세하게는 양극산화막이 형성된 알루미늄의 표면을 직경이 0.4 내지 0.5mm인 철사모를 이용하여 200 내지 300㎏f/mm2의 강도로 1차 회전 연마하고, 직경이 0.1 내지 0.3mm인 철사모를 이용하여 100 내지 150㎏f/mm2의 강도로 2차 회전 연마하는 것이 바람직하다.In more detail, the surface of the aluminum on which the anodization film is formed is first rotationally polished with a strength of 200 to 300 kgf/mm 2 using a wire hair having a diameter of 0.4 to 0.5 mm, and a wire hair having a diameter of 0.1 to 0.3 mm is used. Thus, it is preferable to perform secondary rotary grinding with an intensity of 100 to 150 kgf/mm 2 .
또한, 필요에 따라서는 상기 1차 및 2차 회전 연마를 통해 알루미늄의 표면에 발생한 스크래치 등을 제거하기 위해 직경이 0.01 내지 1mm인 철사모를 이용하여 10 내지 50㎏f/mm2의 강도로 추가적인 연마의 공정을 진행할 수도 있다.In addition, if necessary, additional polishing with a strength of 10 to 50 kgf/mm 2 using wire hair having a diameter of 0.01 to 1 mm in order to remove scratches etc. generated on the surface of aluminum through the first and second rotary polishing may proceed with the process of
상기의 과정을 통해 알루미늄의 표면에 형성되어 있던 불순물과 양극산화막의 일부가 제거되면, 상기 산성분침지단계(S103)를 통해 알루미늄의 표면에 형성된 양극산화막의 제거하는 과정에서 양극산화막의 제거 효과가 월등하게 향상된다.When the impurities formed on the surface of the aluminum and a part of the anodization film are removed through the above process, the removal effect of the anodization film in the process of removing the anodization film formed on the surface of the aluminum through the acidic powder immersion step (S103) is increased. significantly improved
상기 산성분침지단계(S103)는 상기 불순물제거단계(S101)를 통해 불순물이 제거된 알루미늄을 산성분에 침지하여 양극산화막을 제거하는 단계로, 상기 불순물제거단계를 통해 불순물과 양극산화막의 일부가 제거된 알루미늄을 산성분에 4 내지 5시간 동안 침지하여 이루어지는데, 상기와 같이 산성분을 사용하게 되면 알루미늄의 표면에 형성된 양극산화막의 제거효과가 우수하게 나타나면서도 알루미늄의 부식이 억제되어 알루미늄으로 이루어진 제품의 재생작업을 다수 반복하더라도 알루미늄 제품의 치수나 알루미늄 제품에 형성된 홀 등의 크기가 크게 변경되지 않는 효과를 나타낸다.The acidic minute immersion step (S103) is a step of removing the anodized film by immersing the aluminum from which the impurities have been removed through the impurity removal step (S101) in an acidic component to remove the impurities and a part of the anodized film through the impurity removal step. It is made by immersing the removed aluminum in acidic powder for 4 to 5 hours. When the acidic powder is used as described above, the removal effect of the anodized film formed on the surface of aluminum is excellent, and corrosion of aluminum is suppressed, It shows the effect that the size of the aluminum product or the size of the hole formed in the aluminum product does not change significantly even if the product regeneration operation is repeated many times.
또한, 상기 산성분은 pH가 1.5 내지 5.5를 나타내는 것을 사용하는 것이 바람직한데, 상기와 같은 pH범위를 갖는 산성분은 알루미늄의 표면에 형성된 양극산화막의 제거효과가 우수하면서도 알루미늄을 부식시키지 않는 효과를 나타낸다.In addition, it is preferable to use the acid component having a pH of 1.5 to 5.5. The acid component having the above pH range has an excellent effect of removing the anodization film formed on the surface of aluminum and does not corrode aluminum. indicates.
또한, 상기 산성분침지단계(S103)에서 침지시간이 4시간 미만이면 양극산화막의 제거효과가 미미하며, 상기 상성분침지단계(S103)에서 침지시간이 5시간을 초과하게 되면 양극산화막의 대부분이 제거된 후에도 계속적으로 침지과정을 진행하는 것으로 알루미늄의 부식이 진행될 수 있기 때문에 바람직하지 못하다.In addition, if the immersion time is less than 4 hours in the acidic minute immersion step (S103), the removal effect of the anodization film is insignificant, and when the immersion time exceeds 5 hours in the phase component immersion step (S103), most of the anodization film is It is undesirable because corrosion of aluminum may proceed by continuing the immersion process even after removal.
이때, 상기 산성분은 질산, 인산, 황산, 염산, 주석산, 및 옥살산으로 이루어진 그룹에서 선택된 하나 이상이 함유되는 것을 사용하는 것이 바람직하며, 필요에 따라서는 산성수를 사용할 수도 있다.In this case, it is preferable to use the acid component containing at least one selected from the group consisting of nitric acid, phosphoric acid, sulfuric acid, hydrochloric acid, tartaric acid, and oxalic acid, and acidic water may be used if necessary.
상기 알칼리수세척단계(S105)는 상기 산성분침지단계(S103)를 통해 양극산화막이 제거된 알루미늄의 표면을 알칼리수로 세척하는 단계로, 상기 산성분침지단계(S103)를 통해 양극산화막이 제거된 알루미늄의 표면을 알칼리수로 세척하여, 알루미늄의 표면에 잔존하는 산성분을 중화하는 단계다.The alkaline water washing step (S105) is a step of washing the surface of the aluminum from which the anodization film has been removed through the acidic minute immersion step (S103) with alkaline water. It is a step to neutralize the acid content remaining on the surface of aluminum by washing the surface of the aluminum with alkaline water.
이때, 상기 알칼리수는 물을 전기 분해하여 생성된 것으로, 알루미늄 표면의 산성분을 중화 및 세척하는 역할을 하는데, 알칼리수 내에 녹아있는 히드록실이온(H3O2 -)의 소수성기(OH-)가 알루미늄 표면에 잔존하는 산성분을 세척 및 제거하게 된다.At this time, the alkaline water is generated by electrolysis of water, and serves to neutralize and wash the acid content on the surface of aluminum. Hydrophobic groups (OH- ) of hydroxyl ions (H 3 O 2 - ) dissolved in alkaline water are The acid content remaining on the surface is washed and removed.
이때, 상기 알칼리수는 pH가 9 내지 10을 나타내는 것이 바람직하며, 온도는 30 내지 40℃을 나타내는 것이 바람직한데, 알칼리수의 pH가 10을 초과하게 되면 알루미늄의 표면에 잔존하는 산성분을 제거함과 동시에 알루미늄의 표면에서 부식의 과정이 진행되기 때문에 바람직하지 못하다.At this time, the alkaline water preferably has a pH of 9 to 10, and a temperature of 30 to 40° C. When the pH of the alkaline water exceeds 10, the acid content remaining on the surface of aluminum is removed and aluminum It is undesirable because the process of corrosion proceeds on the surface of
또한, 알칼리수세척단계(S105) 이후에는 필요에 따라 알칼리수세척단계(S105)를 통해 알칼라수로 세척된 알루미늄을 정제수로 세척한 후에 건조하는 과정을 진행하는 것이 바람직하다.In addition, after the alkaline water washing step (S105), if necessary, it is preferable to proceed with the drying process after washing the aluminum washed with alkaline water through the alkaline water washing step (S105) with purified water.
또한, 상기 불순물제거단계(S101)와 상기 산성분침지단계(S103) 사이에는 상기 불순물제거단계(S101)를 통해 불순물이 제거된 알루미늄을 산화막 환원제에 침지하는 산화막환원단계(S102)가 더 진행될 수 있는데, 상기와 같이 산화막환원단계(S102)가 더 진행되면 알루미늄의 표면에 형성된 양극산화막이 환원되어 상기 산성분침지단계(S103)에서 양극산화막의 제거효율이 더욱 향상되며, 상기 산화막환원단계(S103)를 거치면 상기 산성분침지단계(S103)에서 알루미늄을 산성분에 침지하는 시간을 줄일 수 있기 때문에 알루미늄의 부식을 최소화 할 수 있을 뿐만 아니라, 산성분침지단계(S103) 이후에 알루미늄의 표면에 녹이 발생하는 것을 억제할 수 있다.In addition, between the impurity removing step (S101) and the acidic partial immersion step (S103), the oxide film reduction step (S102) of immersing the aluminum from which the impurities have been removed in the oxide film reducing agent through the impurity removing step (S101) may be further proceeded. However, when the oxide film reduction step (S102) is further progressed as described above, the anodization film formed on the surface of the aluminum is reduced, so that the removal efficiency of the anodization film in the acidic powder immersion step (S103) is further improved, and the oxide film reduction step (S103) ), it is possible to reduce the time for immersing the aluminum in the acidic powder in the acidic powder immersion step (S103), so that corrosion of aluminum can be minimized, and rust on the surface of aluminum after the acidic powder immersion step (S103) can be prevented from occurring.
상기와 같은 성분으로 이루어지는 산화막 환원제를 이용한 산화막환원단계(S102)가 진행되면, 상기 산성분침지단계(S103)가 2분 내외로 진행되더라도 알루미늄의 표면에 형성된 양극산화막이 대부분 제거될 수 있다.When the oxide film reduction step (S102) using the oxide film reducing agent composed of the above components proceeds, even if the acidic powder immersion step (S103) proceeds for about 2 minutes, most of the anodic oxide film formed on the surface of aluminum can be removed.
이때, 상기 산화막 환원제는 히드라진계 화합물 또는 차인산계 화합물이 0.2 내지 20 중량% 함유되는 것이 바람직하며, 상기 히드라진계 화합물은 히드라진 벤젠, 히드라진 카보네이트, 히드라진 카복시오아마이드, 히드라진 카복사마이드, 히드라진 하이드라이드, 히드라진 브로마이드, 히드라진 클로라이드, 히드라진 설페이드, 히드라진- 에탄올 및 히드라진 살프(Hydrazine salf)로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것이 더욱 바람직하며, 상기 차인산계 화합물은 하이포인산염(K,Na염) 및 하이포아인산으로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것이 바람직하다.In this case, the oxide film reducing agent preferably contains 0.2 to 20% by weight of a hydrazine-based compound or a hypophosphorous acid-based compound, and the hydrazine-based compound includes hydrazine benzene, hydrazine carbonate, hydrazine carboxyamide, hydrazine carboxamide, hydrazine hydride, More preferably, the compound comprises at least one selected from the group consisting of hydrazine bromide, hydrazine chloride, hydrazine sulfate, hydrazine-ethanol and hydrazine salf, and the hypophosphorous acid-based compound is hypophosphate (K, Na salt) and hypophosphorous acid. It is preferable that it consists of one or more selected from the group consisting of.
이하에서는, 본 발명에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법을 실시예를 들어 설명하기로 한다.Hereinafter, a method of removing an anodization film formed on an aluminum surface according to the present invention will be described with reference to an embodiment.
<실시예 1><Example 1>
양극산화막이 형성된 알루미늄을 표면을 직경이 0.5mm인 철사모를 이용하여 250㎏f/mm2의 강도로 1차 회전 연마하고, 직경이 0.2mm인 철사모를 이용하여 125㎏f/mm2의 강도로 2차 회전 연마한 후에 질량농도가 98%인 질산에 4시간 동안 침지하고, 침지가 완료된 후에는 알칼리수(pH 9)로 세척하여 알루미늄 표면에 형성된 양극산화막을 제거하였다.The surface of the aluminum on which the anodization film has been formed is first rotationally polished to a strength of 250 kgf/mm 2 using a wire hair with a diameter of 0.5 mm, and a strength of 125 kgf/mm 2 using a wire hair with a diameter of 0.2 mm. After the second rotation polishing, it was immersed in nitric acid having a mass concentration of 98% for 4 hours, and after immersion was completed, it was washed with alkaline water (pH 9) to remove the anodized film formed on the aluminum surface.
<실시예 2><Example 2>
상기 실시예 1과 동일하게 진행하되, 질산에 4시간 동안 침지하여 알루미늄 표면에 형성된 양극산화막을 제거하였다.The same procedure as in Example 1 was performed, except that the anodic oxide film formed on the aluminum surface was removed by immersion in nitric acid for 4 hours.
<비교예 1><Comparative Example 1>
상기 실시예 1과 동일하게 진행하되, 질산에 1시간 동안 침지하여 알루미늄 표면에 형성된 양극산화막을 제거하였다.The same procedure as in Example 1 was performed, except that the anodic oxide film formed on the aluminum surface was removed by immersion in nitric acid for 1 hour.
<비교예 2><Comparative Example 2>
상기 실시예 1과 동일하게 진행하되, 질산에 2시간 동안 침지하여 알루미늄 표면에 형성된 양극산화막을 제거하였다.The same procedure as in Example 1 was performed except that the anodic oxide film formed on the aluminum surface was removed by immersion in nitric acid for 2 hours.
<비교예 3><Comparative Example 3>
상기 실시예 1과 동일하게 진행하되, 질산에 3시간 동안 침지하여 알루미늄 표면에 형성된 양극산화막을 제거하였다.The same procedure as in Example 1 was performed, except that the anodic oxide film formed on the aluminum surface was removed by immersion in nitric acid for 3 hours.
상기 실시예 1 내지 2 및 비교예 1 내지 3을 통해 양극산화막이 제거된 알루미늄의 단면을 주사전자현미경(SEM)으로 촬영하여 아래 도 3에 나타내었다.Cross-sections of aluminum from which the anodization film was removed in Examples 1 to 2 and Comparative Examples 1 to 3 were photographed with a scanning electron microscope (SEM), and are shown in FIG. 3 below.
아래 도 3에 나타낸 것처럼, 실시예 1 내지 2과 같이 산성분에 4 내지 5시간 동안 침지된 알루미늄은 양극산화막의 두께가 2 내지 3㎛를 나타내어 초기 양극산화막의 두께인 41 내지 46㎛와 비교했을 때, 양극산화막이 대부분 제거된 것을 알 수 있으며, 비교예 1 내지 3과 같이 산성분에 1 내지 3시간 동안 침지된 알루미늄은 양극산화막의 두께가 18 내지 41㎛를 나타내어 양극산화막의 제거효율이 낮은 것을 알 수 있다.As shown in FIG. 3 below, aluminum immersed in acid powder for 4 to 5 hours as in Examples 1 and 2 exhibited a thickness of 2 to 3 μm, compared with 41 to 46 μm, which is the thickness of the initial anodization layer. At this time, it can be seen that most of the anodized film is removed, and as in Comparative Examples 1 to 3, aluminum immersed in acidic powder for 1 to 3 hours has a thickness of 18 to 41 μm, so the removal efficiency of the anodization film is low. it can be seen that
또한, 상기 실시예 1 내지 2 및 비교예 1 내지 3의 과정을 거치면서 알루미늄의 무게 변화를 측정하여 아래 도 4에 나타내었다.In addition, the weight change of aluminum was measured through the processes of Examples 1 to 2 and Comparative Examples 1 to 3 and shown in FIG. 4 below.
아래 도 4에 나타낸 것처럼, 본 발명의 실시예 1 내지 2와 같이 질산에 4 내지 5시간 동안 침지하더라도, 알루미늄의 무게가 0.01% 미만으로 감소되어 부식의 진행이 거의 없는 것을 알 수 있다.As shown in Figure 4 below, even when immersed in nitric acid for 4 to 5 hours as in Examples 1 and 2 of the present invention, the weight of aluminum is reduced to less than 0.01%, so it can be seen that there is hardly any progress of corrosion.
따라서, 본 발명에 따른 알루미늄 표면에 형성된 양극산화막의 제거방법은 알루미늄의 표면에 형성된 양극산화막의 제거효율이 우수할 뿐만 아니라, 알루미늄의 부식을 억제할 수 있다.Accordingly, the method for removing the anodization film formed on the surface of aluminum according to the present invention has excellent removal efficiency of the anodization film formed on the surface of aluminum and can suppress corrosion of aluminum.
S101 ; 불순물제거단계
S102 ; 산화막환원단계
S103 ; 산성분침지단계
S105 ; 알칼리수세척단계S101; Impurity removal step
S102; Oxide reduction step
S103; Acid powder immersion step
S105 ; Alkaline water washing step
Claims (7)
상기 불순물제거단계를 통해 불순물이 제거된 알루미늄을 산성분에 침지하여 양극산화막을 제거하는 산성분침지단계; 및
상기 산성분침지단계를 통해 양극산화막이 제거된 알루미늄의 표면을 알칼리수로 세척하는 알칼리수세척단계;로 이루어지는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
an impurity removal step of removing impurities from the surface of the aluminum on which the anodization film is formed;
an acidic powder immersion step of immersing the aluminum from which impurities have been removed through the impurity removal step in acidic powder to remove the anodized film; and
An alkaline water washing step of washing the surface of the aluminum from which the anodized film has been removed through the acidic minute immersion step with alkaline water;
상기 불순물제거단계는 양극산화막이 형성된 알루미늄의 표면을 철사모로 연마하여 이루어지는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
The method according to claim 1,
The step of removing the impurities is a method of removing an anodized film formed on the surface of aluminum, characterized in that the polishing is made by grinding the surface of the aluminum on which the anodized film is formed with a wire bristles.
상기 철사모는 100 내지 300㎏f/mm2의 강도를 나타내며 0.1 내지 0.5mm의 직경으로 형성되는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
The method according to claim 1,
The wire hair is 100 to 300 kgf / mm 2 Removal of the anodization film formed on the surface of the aluminum, characterized in that it is formed with a diameter of 0.1 to 0.5mm representing a strength of.
상기 산성분침지단계는 4 내지 5시간 동안 이루어지는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
The method according to claim 1,
The method of removing the anodic oxide film formed on the aluminum surface, characterized in that the acid minute immersion step is performed for 4 to 5 hours.
상기 산성분은 pH가 1.5 내지 5.5이며,
질산, 인산, 황산, 염산, 주석산, 및 옥살산으로 이루어진 그룹에서 선택된 하나 이상이 함유되는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
The method according to claim 1,
The acidic component has a pH of 1.5 to 5.5,
A method for removing an anodization film formed on an aluminum surface, characterized in that it contains at least one selected from the group consisting of nitric acid, phosphoric acid, sulfuric acid, hydrochloric acid, tartaric acid, and oxalic acid.
상기 불순물제거단계와 상기 산성분침지단계 사이에는 상기 불순물제거단계를 통해 불순물이 제거된 알루미늄을 산화막 환원제에 침지하는 산화막환원단계가 더 진행되는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.
The method according to claim 1,
Between the impurity removing step and the acidic minute immersion step, an oxide film reduction step of immersing the aluminum from which impurities have been removed through the impurity removing step in an oxide film reducing agent is further performed.
상기 산화막 환원제는 히드라진계 화합물 또는 차인산계 화합물이 0.2 내지 20 중량% 함유되는 것을 특징으로 하는 알루미늄 표면에 형성된 양극산화막의 제거방법.7. The method of claim 6,
The oxidation film reducing agent is a method of removing an anodized film formed on the surface of aluminum, characterized in that 0.2 to 20% by weight of a hydrazine-based compound or a hypophosphorous acid-based compound is contained.
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| KR101362438B1 (en) | 2013-10-02 | 2014-02-13 | (주)아인스 | Method for eliminating aluminum oxide film on aluminum surface and method for regenerating alumimum oxide film including the same |
| KR101625698B1 (en) | 2010-06-23 | 2016-05-30 | 우에무라 고교 가부시키가이샤 | Aluminum oxide film remover and method for surface treatment of aluminum or aluminum alloy |
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| KR101362438B1 (en) | 2013-10-02 | 2014-02-13 | (주)아인스 | Method for eliminating aluminum oxide film on aluminum surface and method for regenerating alumimum oxide film including the same |
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