KR920006044B1 - Surface treating composition - Google Patents
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- KR920006044B1 KR920006044B1 KR1019900011610A KR900011610A KR920006044B1 KR 920006044 B1 KR920006044 B1 KR 920006044B1 KR 1019900011610 A KR1019900011610 A KR 1019900011610A KR 900011610 A KR900011610 A KR 900011610A KR 920006044 B1 KR920006044 B1 KR 920006044B1
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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Abstract
Description
본 발명은 표면처리 조성물에 관한 것으로서, 상세하게는 도금처리하여 형성된 피도금물중 불량한 것을 회수하여 불량피막을 박리시킴으로서 재도금 가능한 표면을 형성하게 하는 개량된 표면처리 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a surface treatment composition, and more particularly, to an improved surface treatment composition for recovering a poor one from a plated product formed by plating to remove a poor coating to form a replatable surface.
일반적으로 티타늄(TI)과 그 합금물질 예컨대, TiN, TiC, TiBr, TiCN, TiS, TiA1 및 TiNi등은 화학증착법(CVD), 플라즈마 CVD법등의 방법에 의해 스테인레스강의 상부에 피복되어 사용되어 왔다.In general, titanium (TI) and its alloying materials, such as TiN, TiC, TiBr, TiCN, TiS, TiA1 and TiNi, have been used by being coated on top of stainless steel by chemical vapor deposition (CVD), plasma CVD, or the like.
이와 같은 방법으로 피복된 Ti합금표면은 기계적 강도, 내마모성 및 내식성이 뛰어날 뿐만 아니라 부가적으로 여러가지 처리방법에 의해 광휘성이 향상되며, 이러한 방법은 절삭공구, 장식기구, 고압용기, 진공용기, 시계부품, 전선 및 반도체등의 정밀산업분야에서 널리 사용되고 있다.The Ti alloy surface coated in this way not only has excellent mechanical strength, abrasion resistance and corrosion resistance, but also additionally improves the brightness by various treatment methods, such as cutting tools, decorative tools, high pressure vessels, vacuum vessels, watches Widely used in the precision industry such as parts, wires and semiconductors.
그러나 이들 방법으로 형성된 피도금물중 약 20∼30%가 불량을 초래하는데 이러한 불량 피도금물은 회수하여 재사용하지 않고 폐기처분 하였으므로, 이로 인한 비용손실은 막대하였다.However, about 20 to 30% of the plated materials formed by these methods cause defects. Since such defective plated materials were collected and disposed of without reuse, the cost loss was enormous.
따라서 폐기처분되는 불량 피도금물을 회수하여 재생처리해서 재도금 가능한 표면을 형성하게 하는 표면처리 조성물이 요망되고 있다.Accordingly, there is a demand for a surface treatment composition that recovers and discards the defective to-be-plated object to form a replatable surface.
지금까지 공지된 표면처리 조성물은 그 성분과 성분비가 정확히 알려져 있지 않았지만 일부 사용되어 온것으로서는 다음과 같은 것이 있다. 예를들어, HNO3,NaNO3및 H2SO4등의 무기산 또는 그의 염을 사용하여 Ti합금피막을 박리시키는 방법이 있는데, 이 방법에 의하면, 소지금속표면이 산에 의해 부식되므로 재사용이 불가능해져서 그로 인한 비용손실이 크다는 문제가 있으며, 또한 TiC와 TiN은 선별적인 박리가 필요하므로 TiC용 및 TiN용 표면처리 조성물이 따로따로 요구되기도 하고, 경우에 따라서는 하나의 용액으로 완전처리되지 않아 다른 용액과 혼합하여 사용해야 한다는 단점도 있다.The surface-treatment compositions known so far have not been known exactly in terms of their components and component ratios, but some of them have been used as follows. For example, there is a method of peeling the Ti alloy film by using an inorganic acid such as HNO 3 , NaNO 3 and H 2 SO 4 , or a salt thereof. According to this method, since the base metal surface is corroded by acid, it cannot be reused. As a result, there is a problem in that the cost loss is large, and since TiC and TiN require selective peeling, surface treatment compositions for TiC and TiN are separately required, and in some cases, they are not completely treated with one solution, Another disadvantage is that it must be mixed with the solution.
즉, 종래의 표면처리 조성물로 스테인레스강 상의 Ti합금피막을 박리하는 경우의 가장 주된 문제점은 소지금속의 표면을 손상시켜 재사용이 불가능해진다는 것이다.That is, the main problem in peeling the Ti alloy film on the stainless steel with the conventional surface treatment composition is that the surface of the base metal is damaged and cannot be reused.
본 발명의 목적은 상기 문제를 감안하여 스테인레스 강판상에 도금된 Ti합금피막중 불량한 것만을 회수하여 원래의 스테인레스 강판의 표면에는 어떠한 손상도 주지 않고 Ti합금만을 완전히 박리하여 재도금이 가능하도록 하는 표면처리 조성물을 제공하는 것이다.It is an object of the present invention to recover only the poor one of the Ti alloy film plated on the stainless steel sheet in view of the above problems and to completely peel only the Ti alloy without any damage to the surface of the original stainless steel sheet to enable replating To provide a treatment composition.
상기 목적을 달성하기 위하여 본 발명에서는, 구연산염 또는 글루콘산염 0.5 내지 20중량%, 구연산 또는 초산 0.5 내지 20중량%, 할로겐염 0.01 내지 10중량%, 산화제 1 내지 15중량%, 양이온계면활성제 0.001내지 10중량% 및 순수를 포함하는 것을 특징으로 하는, 티타늄합금피막이 형성된 스테인레스강으로부터 티타늄합금피막을 박리시키기 위한 표면처리 조성물을 제공한다.In order to achieve the above object, in the present invention, 0.5 to 20% by weight of citrate or gluconate, 0.5 to 20% by weight of citric acid or acetic acid, 0.01 to 10% by weight of halogen salt, 1 to 15% by weight of oxidizing agent, and 0.001 to cationic surfactant The surface treatment composition for peeling a titanium alloy film from the stainless steel in which the titanium alloy film was formed, characterized by including 10 weight% and pure water.
본 발명의 표면처리 조성물중 구연산염 또는 글루콘산염은 금속이온 격리제 및 산성화제로서 첨가되는데, 조성물 총량의 0.5중량% 보다 적으면 그 작용을 나타내지 못하고, 20중량% 보다 많아도 첨가에 따른 효과의 증진이 없으므로 0.5 내지 20중량%로 사용하여야 하며, 2 내지 10중량%가 바람직하다. 구연산염으로는 구연산 나트륨 또는 구연산 칼륨등이 바람직하고, 글루콘산염으로는 글루콘산나트륨 또는 글루콘산칼륨등이 바람직하다.In the surface treatment composition of the present invention, citrate or gluconate is added as a metal ion sequestering agent and an acidifying agent, and when it is less than 0.5% by weight of the total amount of the composition, it does not show its effect, and when it is more than 20% by weight, the effect of addition is enhanced. Since there is no use, 0.5 to 20% by weight should be used, and 2 to 10% by weight is preferable. As citrate, sodium citrate or potassium citrate is preferable, and as gluconate, sodium gluconate or potassium gluconate is preferable.
또한 상기 조성물중 구연산 또는 초산은 산성화제로서, 첨가되는데, 조성물 총량의 0.5중량% 보다 적거나 20중량% 보다 많으면 조성물의 pH가 적절하지 못하며 박리효과가 떨어지거나 또는 소지표면의 손상을 가져오므로 0.5 내지 20중량%로 첨가하여야 하며 2 내지 10중량%가 바람직하다.In addition, citric acid or acetic acid in the composition is added as an acidifying agent, if less than 0.5% by weight or more than 20% by weight of the total composition of the composition is not appropriate pH, the peeling effect or damage to the surface of the base is 0.5 To 20% by weight and 2 to 10% by weight is preferred.
본 발명의 표면처리 할로겐화염은 티타늄합금 피막을 박리시키는 주성분으로서, 조성물 총량의, 0.01중량% 보다 적게 첨가되면 박리효과가 미미하고 10중량% 보다 많아도 첨가에 따른 효과의 증진이 없으므로 0.01 내지 10중량%로 사용하여야 하며, 0.01 내지 5중량%가 바람직하다. 할로겐염으로 일반식 RX(식중 R은 알칼리금속, 알칼리토류금속 또는 NH4를 나타내고 X는 F,Cl,Br 또는 I를 나타낸다)로 표기되는 화합물이 바람직하다.The surface-treated halide salt of the present invention is a main component that peels the titanium alloy film, and when less than 0.01% by weight of the total amount of the composition is added, the peeling effect is insignificant, and even if it is more than 10% by weight, 0.01 to 10% by weight is not enhanced. It should be used in%, preferably 0.01 to 5% by weight. The halogen salt is preferably a compound represented by the general formula RX (wherein R represents an alkali metal, an alkaline earth metal or NH 4 and X represents F, Cl, Br or I).
또한 상기 조성물중 산화제는 본 발명의 표면처리 조성물의 활성화제로서 첨가되는데, 조성물 총량의 1중량% 보다 적게 첨가되면 박리에 요하는 시간이 길어지고, 15중량% 보다 많아도 첨가에 따른 박리시간의 단축이 없으므로 1 내지 15중량% 사용한다. 산화제로는 과산화수소(H2O2) 및 과산화나트륨(Na2O2)과 같은 무기 및 유기과산화물 외에도 중크롬산나트륨(Na2Cr2O7), 과망간산칼륨(KMnO4) 및 과황산암모늄((NH4)2S2O8)과 같은 산화제도 사용될 수 있다.In addition, the oxidizing agent in the composition is added as an activator of the surface treatment composition of the present invention, when less than 1% by weight of the total amount of the composition, the time required for peeling is long, even if more than 15% by weight shortening the peeling time according to the addition Since there is no 1 to 15% by weight. Oxidizers include sodium bichromate (Na 2 Cr 2 O 7 ), potassium permanganate (KMnO 4 ) and ammonium persulfate ((NH) in addition to inorganic and organic peroxides such as hydrogen peroxide (H 2 O 2 ) and sodium peroxide (Na 2 O 2 ) 4 ) Oxidants such as 2 S 2 O 8 ) may be used.
본 발명의 표면처리 조성물에서 양이온계면활성제는 소지금속표면의 부식을 억제시키기 위하여 첨가되며, 조성물 총량의 0.001중량% 보다 적으면 소지의 부식우려가 있으며 10중량% 보다 많아도 첨가에 따른 부식억제효과의 증진이 없으므로 0.001 내지 10중량%로 사용하고, 0.1 내지 3중량%가 바람직하다. 양이농계면활성제로는 4급 암모늄염, 피리디늄염등이 사용되고, 4급 암모늄염중에서는 테트라알킬 암모늄염과 트리알킬벤질 암모늄염이 바람직하다. 테트라알킬암모늄염의 예로는 헥사데실트리메틸암모늄염, 라우릴트리메틸벤질 암모늄염등이 포함되고 피리디늄염의 예로는 도데실피리디늄염등이 포함된다.In the surface treatment composition of the present invention, the cationic surfactant is added to suppress the corrosion of the surface of the base metal, and if it is less than 0.001% by weight of the total amount of the composition, there is a possibility of corrosion of the base and the corrosion inhibitory effect of the addition may be higher than 10% by weight. Since there is no improvement, it is used at 0.001 to 10% by weight, preferably 0.1 to 3% by weight. A quaternary ammonium salt, a pyridinium salt, etc. are used as a bipartite surfactant, A tetraalkyl ammonium salt and a trialkylbenzyl ammonium salt are preferable among quaternary ammonium salts. Examples of tetraalkylammonium salts include hexadecyltrimethylammonium salts, lauryltrimethylbenzyl ammonium salts, and the like, and examples of pyridinium salts include dodecylpyridinium salts and the like.
본 발명의 바람직한 실시예를 설명하면 다음과 같다.Referring to the preferred embodiment of the present invention.
[실시예 1]Example 1
둥근 플라스크에 물 50g과 NH4F 3g, 구연산나트륨 4g, 구연산 6g를 넣고 상온에서 약 1시간동안 교반한다. 여기에 H2O27g를 넣고 4℃에서 30분간 교반한 다음, 자외선에 안정성이 약하므로 갈색병에서 1일간 방치한다. 그후 얻어진 화합물을 상온에서 약 5시간동안 교반하여 양이온 계면활성제 0.5g을 첨가하고 물을 가해 100g으로 한 다음 교반하여 본 발명의 표면처리 조성물을 얻었다.In a round flask, 50 g of water, NH 4 F 3 g, sodium citrate 4 g, and citric acid 6 g were added and stirred at room temperature for about 1 hour. 7 g of H 2 O 2 was added thereto and stirred at 4 ° C. for 30 minutes, and then left in a brown bottle for 1 day because of poor stability to ultraviolet rays. Thereafter, the obtained compound was stirred at room temperature for about 5 hours to add 0.5 g of a cationic surfactant, to 100 g by adding water, and then stirred to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물에 두께 2mm의 스테인레스강(10×10) 표면위에 2mm 두께로 Ti합금을 피복시킨 시료를 1분간 실온에서 함침하여 처리한 다음 꺼내어 육안 및 현미경으로 확인한 바, 스테인레스강 소지에는 전혀 손상을 주지 않고 Ti합금만을 완전히 박리하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.The composition obtained in this manner was impregnated with a sample coated with a Ti alloy with a thickness of 2 mm on a stainless steel (10 × 10) surface having a thickness of 2 mm at room temperature for 1 minute, then taken out and checked by naked eye and a microscope. It was found that only the Ti alloy was completely peeled off without any damage. The results are shown in Table 1.
[실시예 2]Example 2
상기 실시예 1과 동일하게 시행하되 구연산 대신 초산 3g과 과산화수소 대신 Na2O23g을 사용하고, 10-2torr에서 진공교반기를 이용하여 18시간동안 교반하여 본 발명의 표면처리 조성물을 얻었다.In the same manner as in Example 1, but using 3g of acetic acid instead of citric acid and 3g of Na 2 O 2 instead of hydrogen peroxide, and stirred for 18 hours using a vacuum stirrer at 10 -2 torr to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.8% 박리하는데 30분 소요하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.The peeling test of the composition thus obtained in the same manner as in Example 1 showed that it took 30 minutes to peel 99.8%. The results are shown in Table 1.
[실시예 3]Example 3
삼각플라스크에 물 50g과 NH4F 4g, 글르콘산나트륨 5g을 넣고 약 30℃에서 5분간 가열하고 상온으로 냉각시킨 후 초산 3g을 계속하여 넣고 4시간동안 교반한다. 그후 약 42시간동안 냉암소에 보관한 후 Na2O24g과 양이온 계면활성제 소량을 첨가하고 물을 가해 100g으로 한 다음 교반하여 본 발명의 표면처리 조성물을 얻었다.Add 50g of water, NH 4 F 4g, and sodium gluconate 5g to the Erlenmeyer flask, heat at about 30 ° C for 5 minutes, cool to room temperature, and continue adding 3g of acetic acid for 4 hours. Thereafter, the resultant was stored in a cool dark place for about 42 hours, and then 4 g of Na 2 O 2 and a small amount of a cationic surfactant were added, water was added to 100 g, and stirred to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.8% 박리하는데 35분 소요하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.The peeling test of the composition thus obtained in the same manner as in Example 1 showed that it took 35 minutes to peel 99.8%. The results are shown in Table 1.
[실시예 4]Example 4
둥근 플라스크에 물 5g과 NH4F lg, 구연산나트륨 3g 및 구연산 4g을 혼합한 후 물중탕으로 약 24시간동안 교반한다. 여기에, H2O25g과 양이온 계면활성제 소량을 넣고 물을 가해 100g으로 한 다음 진공하에서 교반 혼합하여 본 발명의 표면처리 조성을을 얻었다.In a round flask, 5 g of water, NH 4 F lg, 3 g of sodium citrate, and 4 g of citric acid are mixed, followed by stirring in a water bath for about 24 hours. 5 g of H 2 O 2 and a small amount of a cationic surfactant were added thereto, water was added to make 100 g, and then stirred and mixed under vacuum to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.8% 박리하는데 30분 소요하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.The peeling test of the composition thus obtained in the same manner as in Example 1 showed that it took 30 minutes to peel 99.8%. The results are shown in Table 1.
[실시예 5]Example 5
삼각플라스크에 물 50g과 NaF 2g, 구연산나트륨 3g 및 구연산 4g을 혼합하여 10-2torr에서 약 3시간동안 교반한 후 물중탕하에서 H2O25g과 양이온 계면활성제 4g을 넣고 물을 가해 100g으로 한 다음 고속교반하여 본 발명의 표면처리 조성물을 얻었다.Erlenmeyer flask, a mixture of water and 50g NaF 2g, 3g of sodium citrate and citric acid 4g After stirring at 10 -2 torr for about 3 hours into the H 2 O 2 5g and cationic surfactants 4g under the water bath add water to 100g After high speed stirring, the surface treatment composition of the present invention was obtained.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.8% 박리하는데 25분 소요하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.The peeling test of the composition thus obtained in the same manner as in Example 1 showed that it took 25 minutes to peel 99.8%. The results are shown in Table 1.
[실시예 6]Example 6
둥근 플라스크에 물 50g과 NaF 2g, 글루콘산나트륨 5g 및 초산 3g을 넣고 감압하에서 혼합하여 1일간 방치한다. 그후 물중탕하에서 H2O25g과 양이온 계면활성제 소량을 넣고 물을 가해 100g로 한 다음 고속혼합하여 본 발명의 표면처리 조성물을 얻었다.50 g of water, 2 g of NaF, 5 g of sodium gluconate, and 3 g of acetic acid were added to a round flask, mixed under reduced pressure, and allowed to stand for 1 day. Subsequently, 5 g of H 2 O 2 and a small amount of cationic surfactant were added thereto under water bath, water was added thereto to make 100 g, and then mixed at a high speed to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.8% 박리하는데 40분 소용하였음을 알 수 있었다. 그 결과를 표 l에 나타내었다.As a result of the peeling test of the composition obtained in the same manner as in Example 1, it was found that 40 minutes was used to peel 99.8%. The results are shown in Table l.
[실시예 7]Example 7
삼각플라스크에 물 50g과 CaF23g, 글루콘산나트륨 5g, 무수초산 2g과 에틸알코올 1g을 넣고 약 50℃에서 5시간동안 저속으로 교반한다. 여기에 Na2O25g과 양이dm온 계면활성제 5g을 넣고 물을 가해 100g으로한 다음 1일간 방치후 냉암 교반하여 본 발명의 표면처리 조성물을 얻었다.50 g of water, 3 g of CaF 2 , 5 g of sodium gluconate, 2 g of acetic anhydride, and 1 g of ethyl alcohol were added to the Erlenmeyer flask, and the mixture was stirred at about 50 ° C. for 5 hours at low speed. 5 g of Na 2 O 2 and 5 g of a positive dm-on surfactant were added thereto to make 100 g of water, and then left to stand for 1 day, followed by cold stirring to obtain a surface treatment composition of the present invention.
이와 같이 하여 얻어진 상기 조성물을 실시예 1과 동일한 방법으로 박리시험을 실시한 결과 99.9% 박리하는데 60분 소요하였음을 알 수 있었다. 그 결과를 표 1에 나타내었다.As a result of performing a peeling test on the composition thus obtained in the same manner as in Example 1, it was found that it took 60 minutes to peel 99.9%. The results are shown in Table 1.
[표 1]TABLE 1
표 1로서, 본 발명의 표면처리 조성물은 1 내지 60분내에 스테인레스강 소지표면에는 전혀 손상을 주지 않고 피복된 Ti합금만을 99.8 내지 99.9% 박리하였음을 알 수 있다.As shown in Table 1, it can be seen that the surface treatment composition of the present invention peeled only 99.8 to 99.9% of the coated Ti alloy without causing any damage to the stainless steel base surface within 1 to 60 minutes.
이상에서 설명한 바와 같이, 본 발명에 의하면 불량 피도금물을 회수하여 소지금속표면에는 전혀 손상을 주지 않고 불량 Ti합금피막을 박리시킴으로써 재도금 가능한 표면을 형성하게 하는 표면처리 조성물을 제공하므로, 종래의 소지금속의 부식을 완전히 방지할 수 있을 뿐 아니라 박리시간을 1분 까지도 단축할 수 있어 생산비를 절감할 수 있게 된다. 게다가 종래 선별적인 박리를 요하던 것도 하나의 용액에서 Ti합금 모두를 박리할 수 있게 되며, 취급이 용이하고 작업환경을 개선시킬 수 있으므로, 본 발명은 장래 공업적 이용가치가 큰 것으로 기대된다.As described above, according to the present invention, there is provided a surface treatment composition which recovers a defective plated material and forms a replatable surface by peeling the defective Ti alloy film without damaging the base metal surface at all. Not only can the corrosion of the base metal be completely prevented, but the peeling time can be shortened to 1 minute, thereby reducing the production cost. In addition, it is expected that the present invention is expected to have a large industrial use value in the future, since the conventional selective peeling can peel all of the Ti alloys in one solution, and can easily handle and improve the working environment.
Claims (5)
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| KR1019900011610A KR920006044B1 (en) | 1990-07-30 | 1990-07-30 | Surface treating composition |
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| KR1019900011610A KR920006044B1 (en) | 1990-07-30 | 1990-07-30 | Surface treating composition |
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