KR100785989B1 - Manufacturing method of lubricant inorganic pre-phosphates coated galvanized steel sheet having a high formability and the steel sheet thereof - Google Patents
Manufacturing method of lubricant inorganic pre-phosphates coated galvanized steel sheet having a high formability and the steel sheet thereof Download PDFInfo
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Abstract
Description
도 1은 윤활제 성상과 부착량의 증가에 마찰계수 측정값을 나타내는 그래프.1 is a graph showing the coefficient of friction measurement to the increase in lubricant properties and adhesion amount.
도 2는 윤활제 성상 부착량에 따른 성형비를 나타내는 그래프.2 is a graph showing the molding ratio according to the lubricant property adhesion amount.
도 3은 윤활제 성상과 부착량에 따른 용접성을 나타내는 그래프.3 is a graph showing the weldability according to the lubricant properties and adhesion amount.
본 발명은 표면윤활성 및 용접성이 우수한 무기인산염계 윤활처리 GA강판(Galvannealed Steel, 합금화 용융아연도금강판)의 제조방법 관한 것이다.The present invention relates to a method for producing an inorganic phosphate lubricated GA steel plate (Galvannealed Steel, alloyed hot dip galvanized steel sheet) excellent in surface lubricity and weldability.
자동차 외판용 강판으로 현재 널리 사용되고 사용량이 날로 증가하고 있는 합금화 용융아연도금강판은 순수한 용융아연 도금 강판의 단점인 용접성과 도장성을 보완하기 위해 도금층을 응고 직전에 재가열 (500~550℃) 하므로써 표면에 옅은 회백색의 철-아연 합금층을 생성시킨 철 합금으로 구성되어 있다. 이 합금화 용융 아연도금강판은 아연부착량이 뛰어나 드로잉 등의 가공을 받아도 도금층 박리가 적고, 부식 및 용접성에서도 용융아연 도금강판에 비해 뛰어나다. 그러나 자동차 외판 등의 고성형 부위의 프레스 심가공시 크랙이 자주 발생하는 문제를 가지고 있어서, 가공성의 개선이 요구되어지고 있다.The alloyed hot-dip galvanized steel sheet, which is widely used for automobile exterior plates and is increasingly used, is reheated (500 ~ 550 ℃) just before solidification of the coating layer to compensate for weldability and paintability, which is a disadvantage of pure hot-dip galvanized steel. It consists of an iron alloy that produces a light gray-white iron-zinc alloy layer. The alloyed hot-dip galvanized steel sheet has a high zinc adhesion amount, so that even when subjected to drawing or the like, the peeling of the plating layer is less, and the corrosion and weldability are superior to the hot-dip galvanized steel sheet. However, there is a problem that cracks frequently occur during deep press forming of high-molded parts such as automobile shells, and workability is required to be improved.
이에 따라 가공성 개선을 위해 연신률이 높은 특수성분 등을 함류한 고급강을 사용할 수 있지만, 이는 제품 가격을 상승시키는 요인으로 작용한다. 따라서, 자동차 외판 등의 고성형 부위를 통상 사용되고 있는 일반강으로 사용하면서도 가공성을 향상시킬 수 있는 방법의 하나로 강판에 윤활처리를 실시하는 방법이 제한되고 있다. 윤활처리 강판은 유기계, 유무기계 혼합형, 무기계 등으로 구분할 수 있는데, 내식성 및 가공성을 향상시키고저 고분자 수지를 기반으로 하는 왁스(wax) 계열 윤활제 및 각종 첨가제로 구성이 되는 유기, 유무기 타입의 윤활처리강판은 프레스 가공 시 크랙 발생빈도가 빈번하여 가공성 개선이 요구된다. 또한, 자동차 차체 용접시 표면처리된 윤활제가 고온, 고압의 용접조건에서 산화되어 탄화물을 형성하여 용접봉에 응착된다. 응착된 탄화물은 전류의 흐름을 방해하여 결국 용접봉의 수명을 떨어뜨리는 현상을 나타내므로 이러한 현상발생을 방지하기 위한 요구가 있어왔다. Accordingly, it is possible to use high-grade steel containing special components with high elongation to improve workability, but this increases the price of the product. Therefore, the method of lubricating a steel plate is limited as one of the methods which can improve workability, even using high forming parts, such as an automobile outer shell, as a general steel used normally. Lubricated steel sheet can be classified into organic, organic / inorganic mixed type, inorganic type, etc., which improves corrosion resistance and processability, and is composed of wax-based lubricant and various additives based on low polymer resin. Treated steel sheet is required to improve the workability due to the frequent occurrence of cracks during press working. In addition, during the welding of the vehicle body, the surface-treated lubricant is oxidized under high temperature and high pressure welding conditions to form carbides and adheres to the electrode. Since the bonded carbide exhibits a phenomenon of interrupting the flow of electric current and eventually decreasing the life of the electrode, there is a demand for preventing such occurrence.
따라서, 본 발명은 위와 같은 문제를 해결하고자 특히 강판의 가공성 향상효과에 주안점을 둔 무기인산염계로 윤활처리강판에 착안한 것이다. 이 윤활처리제의 경우 종래의 것에 비해 가공성을 크게 향상시킴은 물론, 용접시에 탄화물 생성이 없어서 용접봉 수명을 단축시키지 않고, 따라서 연속 용접성을 떨어뜨리지 않는다. 또한 본 윤활처리제 용액은 결정질과 비정질 아연의 복합생성물을 생성하여 GA강판과의 윤활밀착성이 뛰어나고, 자동차 차체 용접 후 탈지 시에 소량의 균일한 결정질의 인산염이 GA강판 표면에 남아, 전착도장의 후처리 공정에서 균일한 인산염조직을 형성시키는 결정핵으로 작용하는 역할을 하여 이후 도장공정에서도 양호한 표면조직을 형성시키는 역할을 한다.Therefore, the present invention focuses on the lubricated steel sheet with an inorganic phosphate system, which focuses on the effect of improving the workability of the steel sheet, in order to solve the above problems. In the case of this lubricating agent, the workability is greatly improved as compared with the conventional one, and there is no carbide generation at the time of welding, which does not shorten the welding rod life and thus does not reduce the continuous weldability. In addition, this lubricating agent solution produces a composite product of crystalline and amorphous zinc, so it has excellent lubrication adhesiveness with GA steel sheet, and a small amount of uniform crystalline phosphate remains on the surface of GA steel sheet during degreasing after welding of automobile body. It acts as a crystal nucleus to form a uniform phosphate structure in the treatment process, thereby forming a good surface texture in the subsequent coating process.
즉, 본 발명에서는 전술한 바와 같이 적절한 구성으로 된 무기인산염계 윤활처리제를 강판, 특히 자동차용 GA강판에 본 발명 윤활처리제를 도포·소부처리하므로써 제조되는 자동차용 GA강판이 프레스 심가공시 파단이 발생되지 않고, 이후 차체 용접 시 연속공정 중에 용접성이 저하되지 않으며, 전착도장의 후처리 시에도 기존 표면처리가 없는 양호한 표면특성을 갖도록 하는데 목적이 있다.That is, in the present invention, the GA sheet for automobiles manufactured by applying and baking the present invention lubricating agent to a steel sheet, in particular, an automobile GA steel sheet, is fractured during press deep processing. It does not occur, since the weldability does not deteriorate during the continuous process when welding the body, there is a purpose to have a good surface characteristics without the existing surface treatment even in the post-treatment of electrodeposition coating.
상기 목적을 달성하기 위하여 본 발명에서는 요구되는 최적의 물성을 갖는 윤활처리GA강판을 생산하기 위한 윤활처리제의 기본물성 및 작업조건 등에 초점을 두고 장기간의 연구와 시험 끝에 고품질의 자동차용 GA(합금화 용융아연도금)강판의 제조가 가능하기에 이르렀다.In order to achieve the above object, the present invention focuses on the basic properties and working conditions of the lubricating agent for producing a lubricated GA steel sheet having the optimum physical properties required. Galvanized) steel sheet can be manufactured.
본 윤활처리 강판의 윤활제 성상을 간단히 설명하면 순수 70~90% 중량부에 윤활성 및 도막 형성을 부여하기 위해 무기 인산염계의 인산아연, 인산을 각각 1~10%중량부, 계 2~20%중량부를 가한다. 여기에서 1%미만이면 도막 밀착성이 저하되고 고른 도막 형성이 안되며 10%를 초과하면 용액안정성이 저하되며 윤활성도 저하된다. 또한, 습윤제(wetting)로서 친수성 계면활성제 0.1~5% 중량부를 가하여 혼합한다. 0.1%미만일 정도로 너무 적으면 입자의 응집으로 인해 윤활성이 떨어지고, 도막 표면에 얼룩이 발생 되기 쉬우며, 5%를 초과하면 윤활피막과 강판 사이의 접착도가 떨어진다. 이 계면활성제는 윤활제를 분산시켜주는 역할을 한다. 또한 윤활성 및 용액안정성을 위해 질산아연, 질산니켈 중 1종 이상을 0.1~5% 중량부로 첨가한 후 용해 혼합하고 고형분이 10~30% 되도록 윤활처리제 용액을 제조한다. 상기 질산아연, 질산니켈 1종 이상의 첨가에 있어 0.1%미만이면 윤활성이 저하되고, 5%를 초과하면 용액안정성이 저하된다. Briefly explaining the lubricant properties of the lubricated steel sheet, in order to give lubricity and coating film formation to 70 to 90% by weight of pure water, 1 to 10% by weight of inorganic phosphate zinc and phosphoric acid, and 2 to 20% by weight of phosphoric acid, respectively. Add wealth If less than 1%, the coating film adhesion is reduced, evenly formed coating film is not formed, if it exceeds 10%, the solution stability is lowered and the lubricity is also lowered. In addition, 0.1 to 5% by weight of a hydrophilic surfactant is added and mixed as a wetting agent. If the amount is less than 0.1%, the lubricity decreases due to the aggregation of particles, and the surface of the coating film is easily stained. If the amount exceeds 5%, the adhesion between the lubricant film and the steel sheet is reduced. This surfactant serves to disperse the lubricant. In addition, for lubrication and solution stability, at least one of zinc nitrate and nickel nitrate is added in an amount of 0.1 to 5% by weight, followed by dissolution and mixing to prepare a lubricating agent solution so that the solid content is 10 to 30%. In the addition of one or more of the above zinc nitrate and nickel nitrate, the lubricity falls below 0.1%, and the solution stability falls below 5%.
이렇게 제조된 무기인산염계 윤활처리제 용액을 연속용융아연도금설비(CGL)를 거친 GA강판에 부착량이 400~1200mg/m2 가 되도록 도포하고, 강판 온도 60~200℃ 범위에서 소부처리함을 포함하는 가공성 및 용접성이 우수한 강판 표면처리 방법이 제공된다. 윤활처리 부착량이 400mg/m2 미만이 되면 강판표면에 윤활성 향상 효과가 크지 않고, 부착량이 1200mg/m2 이상이 되면 오히려 윤활성이 저하된다. 그리고, 건조온도는 60℃ 미만일 경우는 건조가 잘 되지 않으며, 200℃가 넘을 경우는 소재 자체 물성에 영향을 미치므로 60~200℃ 범위에서 관리하는 것이 바람직하다.The inorganic phosphate-based lubricating agent solution thus prepared is applied to the GA steel sheet subjected to the continuous hot dip galvanizing facility (CGL) so as to have an adhesion amount of 400 to 1200 mg / m 2, and to be baked at a steel sheet temperature of 60 to 200 ° C. Provided is a method for surface treatment of steel sheet excellent in workability and weldability. When the lubricated coating weight of less than 400mg / m 2 is not greater the lubricity improving effect on the surface of the steel sheet, when the coating weight is more than 1200mg / m 2 Rather, the lubricity deteriorates. And, if the drying temperature is less than 60 ℃ do not dry well, if it exceeds 200 ℃ it is preferable to manage in the 60 ~ 200 ℃ range because it affects the material properties.
전술한 바와 같이 윤활처리용액은 결정질과 비정질아연의 복합생성물을 생성하여 GA강판과의 윤활밀착성을 현저히 향상시킨다. 보다 상세히 설명하면 델타상의 갈바닐(galvanneal) 표면 위에 결정질과 비정질아연인산염(zinc phosphate) 복합 생성물이 생성되고, 이 복합생성물 층은 경계면 윤활효과(boundary lubrication)를 가져오므로써 강판과 다이면을 분리시켜 다이에 직접 접촉되는 강판의 표면적을 줄여주는 기능을 발휘한다.As described above, the lubrication solution produces a composite product of crystalline and amorphous zinc, which significantly improves lubrication adhesion with the GA steel sheet. In more detail, a crystalline and amorphous phosphate complex is formed on the delta galvanneal surface, and the composite layer has a boundary lubrication to separate the steel sheet and the die face. This reduces the surface area of the steel sheet in direct contact with the die.
도 1은 강판에 도포 되는 윤활제의 부착량과 마찰계수 사이의 상관관계를 도시한 것이다. 도 1에서 알 수 있는 바와 같이 유무기계윤활제, 무기금속산화물계 윤활제에 비해 무기인산염계 윤활제가 일반적으로 마찰계수가 낮아 윤활성을 높여주는 것을 알 수 있고, 특히 그 부착량이 400~1200mg/m2, 특히 600mg/m2 부근에서 가장 양호한 윤활성을 나타내고 있음을 알 수 있다. 이와 같이 윤활제의 적정 범위량으로의 부착량 조절은 경제적인 면과 더불어 효율적인 윤활성을 얻는데 매우 중요하다.1 shows a correlation between the adhesion amount of the lubricant applied to the steel sheet and the friction coefficient. As can be seen in FIG. 1, inorganic phosphate-based lubricants generally have low friction coefficients to improve lubricity compared to non-machine lubricants and inorganic metal oxide-based lubricants. In particular, the adhesion amount is 400 to 1200 mg / m 2 , In particular, it can be seen that the best lubricity is shown in the vicinity of 600 mg / m 2 . As such, adjusting the adhesion amount of the lubricant to an appropriate range amount is very important for obtaining economical efficiency and lubricating property.
도 2는 강판에 도포되는 윤활제의 부착량과 성형비와의 상관관계도 이다.2 is a correlation diagram between the adhesion amount of the lubricant applied to the steel sheet and the molding ratio.
성형비(%) 역시 400~1200mg/m2의 범위에서 양호해지며, 특히 본 발명상의 무기인산염의 경우 600~1000mg/m2부착량 범위에 있을 때가 가장 양호한 것임이 나타나 있다.Molding ratio (%) is also good in the range of 400 ~ 1200mg / m 2 , in particular for the inorganic phosphate of the present invention is shown to be the best when in the range of 600 ~ 1000mg / m 2 deposition amount.
도 3은 강판에 도포 되는 윤활제의 부착량과 용접성과의 상관관계도 이다.3 is a correlation diagram of the adhesion amount and weldability of the lubricant applied to the steel sheet.
용접성은 연속용접 타점수로 나타나 있는데, 용접성은 윤활제 부착량과는 비례하지 않고 비교적 일정한 수준으로 유지됨을 알 수 있으므로, 따라서, 윤활제 부착량이 적을수록 경제적임을 알 수 있다. The weldability is shown by the continuous welding RBI, and it is understood that the weldability is maintained at a relatively constant level, not proportional to the amount of lubricant deposition, and therefore, the smaller the amount of lubricant deposition is, the more economic it is.
이하, 본 발명의 실시예에 대하여 상세히 설명한다. Hereinafter, embodiments of the present invention will be described in detail.
[실시예 1]Example 1
인산, 인산아연이 각각 5%, 계면활성제 2%, 질산아연/질산니켈 2%가 첨가되고 순수로 희석한 무기인산염계(Pre-phosphate) 윤활처리제 용액을 고형분이 10~30% 되도록 제조하였다. 5% phosphoric acid, zinc phosphate, 2% surfactant, 2% zinc nitrate / nickel nitrate were added, and a pure phosphate lubricating agent solution diluted with pure water was prepared to have a solid content of 10-30%.
제조된 윤활처리제 용액을 아연부착량 48g/m2, 두께 0.7t, 가공용 EQ 급 소재 강판에 건조부착량 200~1400mg/m2 이 되도록 도포하고 건조하여 제조하고 다음과 같이 피막 특성을 평가하였으며, 그 결과를 하기표 1에 기재하였다.The lubricating agent solution prepared was coated and dried to a dry adhesion amount of 200 to 1400 mg / m 2 on a zinc coating amount of 48 g / m 2 , thickness 0.7t, and an EQ grade steel sheet for processing, and the film properties were evaluated as follows. Are listed in Table 1 below.
각 특성별 평가기준은 다음과 같았다. Evaluation criteria for each characteristic were as follows.
마찰특성Friction characteristics
마찰특성 평가는 강판을 30x250mm 크기로 절단한 후 마찰계수 측정장비를 이용하여 측정한다. 강판을 다이에 고정시킨 후 강판표면에 10x30mm 면적을 갖는 비드(Bead)를 이용하여 일정압력을 가하여 끌어당겼을 때 인발하중을 측정하여, 면압과 인발하중으로부터 마찰계수를 산출하여 비교하여 평가하였다. 이때의 평가 기준은 마찰계수 ◎: 0.130 미만, ○: 0.140미만, △: 0.150미만, ×: 0.150 이상으로 하였다.Evaluation of friction characteristics is measured by using a coefficient of friction measuring equipment after cutting the steel plate to 30x250mm size. After the steel plate was fixed to the die, the pull load was measured by applying a constant pressure to the steel plate surface using a bead having a 10 × 30 mm area, and the friction coefficient was calculated from the surface pressure and the pull load. The evaluation criteria at this time were made into friction coefficient (circle): less than 0.130, (circle): less than 0.140, (triangle | delta): less than 0.150, and x: 0.150 or more.
가공성Machinability
가공성 평가는 강판을 98mmΦ 절단한 후 컵드로잉을 수행하여 성형비를 구하였다. 이때의 성형비는 다음과 같은 식으로 정의된다. Evaluation of workability was obtained by cutting the steel sheet 98mmΦ and performing cup drawing to determine the molding ratio. The molding ratio at this time is defined by the following equation.
성형비(%)=100(%)-(윤활처리한 강판의 최대 펀치 하중/윤활처리하지 않은 강판의 최대 펀치 하중)×100(%) 이때의 평가기준은 다음과 같았다.Molding ratio (%) = 100 (%)-(maximum punch load of the lubricated steel sheet / maximum punch load of the non-lubricated steel sheet) x 100 (%) The evaluation criteria at this time were as follows.
가공성(성형비) ◎: 9%이상, ○: 6%이상, △: 4% 이상, ×: 4% 미만Workability (molding ratio) ◎: 9% or more, ○: 6% or more, △: 4% or more, ×: less than 4%
용접성 Weldability
용접성 평가는 정치식 점용접기로 전류는 10~11kA, 가압력은 300kgf, 12사이클의 조건으로 연속용접성 평가를 수행하였다. 매회 50타점 간격으로 형성된 너겟의 크기를 측정하여 그 지름이 4√t 이하로 떨어지는 시점을 연속용접성의 값으로 하였다. Weldability evaluation was performed with a stationary spot welder to evaluate the continuous weldability under the conditions of 10 ~ 11kA, pressure of 300kgf and 12 cycles. The size of the nugget formed every 50 RBI intervals was measured and the time when the diameter fell below 4√t was set as the value of continuous weldability.
도장물성Paint property
장물성은 윤활강판의 표면에 전착도장처리를 실시하여 평가하는데, 먼저 전착도장 전처리인 인산염 처리를 행한 후, 기존 무처리 GA강판과 동일한 인산염 결정크기를 갖는지 평가하였다. 또한 전착도장한 강판은 내수밀착성 및 도장내식성 평가를 각각 실시한다.The property properties were evaluated by electrodeposition coating treatment on the surface of the lubricated steel sheet. First, the phosphate treatment, which was pre-deposition coating treatment, was performed, and then the same phosphate crystal size as the existing untreated GA steel sheet was evaluated. In addition, the electrodeposited steel sheets are subjected to the evaluation of water resistance and paint corrosion resistance, respectively.
연속용접 타점수 ◎: 1000타점 이상, ○: 700타점 이상, △: 300타점 이상, ×: 300타점 미만Continuous welding RBI number ◎: More than 1000 RBI, ○: More than 700 RBI, △: More than 300 RBI, ×: Less than 300 RBI
아래의 표 1은 그 결과를 나타낸 것이다Table 1 below shows the results.
상기 표 1의 결과를 발명예와 비교예를 구분하여 상세히 설명하면 다음과 같다.The results of Table 1 are described in detail by dividing the invention example and the comparative example as follows.
인산아연, 인산, 그리고 친수성 계면활성제, 질산아연, 질산니켈 등을 첨가 한 무기인산염계 윤활처리 용액을 제조하여 코팅처리한 본 발명의 무기인산염계 윤활처리 강판은 상기 표 1과 같이 윤활부착량에 따라 물성의 차이를 나타내는데 어떤 경우이든 적정한 부착량(400~1200mg/m2)에서 우수한 물성을 나타냄을 알 수 있다.The inorganic phosphate-based lubricated steel sheet of the present invention prepared and coated with an inorganic phosphate-based lubricated solution added with zinc phosphate, phosphoric acid, and a hydrophilic surfactant, zinc nitrate, nickel nitrate, etc., according to the lubrication amount shown in Table 1 above. In any case, it can be seen that it shows excellent physical properties at an appropriate adhesion amount (400 ~ 1200mg / m 2 ).
비교예-무기금속산화물계를 보면, 금속산화물계의 윤활제와 계면활성제, 폴리비닐계 첨가제 등을 첨가한 무기금속산화물계의 윤활처리 강판은 용접성에서는 우수한 특성은 나타내었으나, 가공성의 정도를 나타내는 마찰특성과 성형성에서는 무기인산염계에 비해 비교 열위에 있음을 알 수 있다.Comparative Example-Inorganic metal oxides, lubricated steel sheets of inorganic metal oxides containing metal oxide lubricants, surfactants, polyvinyl additives, and the like showed excellent properties in weldability, but showed friction in terms of workability. It can be seen that the characteristics and formability are inferior to the inorganic phosphate type.
또한, 비교예-유무기계를 보면, 아크릴레진 수지, 왁스 첨가제의 유무기계 혼합형 윤활처리강판은 상기 무기계인산염 타입의 윤활처리 강판의 성형성 및 용접성에비해, 일층 열세에 있음을 알 수 있다.In addition, in the comparative example-free machine, it can be seen that the machine-mixed lubricated steel sheet having an acrylic resin resin and a wax additive is inferior to the moldability and weldability of the phosphate-type lubricated steel sheet.
본 발명에 의해 GA강판이 프레스 심가공시 파단이 발생되지 않고, 차체용접시 연속공정 중에도 용접성이 저하되지 않으며, 전착도장 후 처리시에도 윤활성이 양호한 표면 특성을 갖도록 하여주고, 아울러 경제적으로도 양호한 결과를 가져다줌을 알 수 있다.According to the present invention, the GA steel sheet does not cause breakage during press deep processing, weldability does not decrease even during continuous process during body welding, and has good lubricity even after treatment after electrodeposition coating, and economically good. You can see that it brings a result.
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| JPS6417880A (en) * | 1987-07-10 | 1989-01-20 | Itarubondaa Spa | Composition for protecting surface of steel from air oxidation |
| KR20010015193A (en) * | 1999-07-08 | 2001-02-26 | 에모토 간지 | Perforative corrosion resistant galvanized steel sheet |
| JP2001059182A (en) | 1999-08-20 | 2001-03-06 | Japan Aviation Electronics Industry Ltd | Rust preventive treating method for galvanizing |
| KR20010106235A (en) * | 2000-05-15 | 2001-11-29 | 후지이 히로시 | Metal surface-treating method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS6417880A (en) * | 1987-07-10 | 1989-01-20 | Itarubondaa Spa | Composition for protecting surface of steel from air oxidation |
| KR20010015193A (en) * | 1999-07-08 | 2001-02-26 | 에모토 간지 | Perforative corrosion resistant galvanized steel sheet |
| JP2001059182A (en) | 1999-08-20 | 2001-03-06 | Japan Aviation Electronics Industry Ltd | Rust preventive treating method for galvanizing |
| KR20010106235A (en) * | 2000-05-15 | 2001-11-29 | 후지이 히로시 | Metal surface-treating method |
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