KR20200076477A - Pickling method of austenitic stainless pipe - Google Patents

Pickling method of austenitic stainless pipe Download PDF

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KR20200076477A
KR20200076477A KR1020180165604A KR20180165604A KR20200076477A KR 20200076477 A KR20200076477 A KR 20200076477A KR 1020180165604 A KR1020180165604 A KR 1020180165604A KR 20180165604 A KR20180165604 A KR 20180165604A KR 20200076477 A KR20200076477 A KR 20200076477A
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stainless steel
austenitic stainless
steel pipe
pickling
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KR1020180165604A
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Korean (ko)
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김영호
이정희
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주식회사 포스코
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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
    • C23G1/08—Iron or steel
    • C23G1/085—Iron or steel solutions containing HNO3
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • 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
    • C23G1/08—Iron or steel
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • C23G3/00—Apparatus for cleaning or pickling metallic material
    • C23G3/04—Apparatus for cleaning or pickling metallic material for cleaning pipes
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/001—Austenite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The present invention provides a method for pickling an austenitic stainless steel pipe having excellent corrosion resistance by optimizing hydrofluoric acid concentration for pickling treatment of the austenitic stainless steel pipe. The method for pickling an austenitic stainless steel pipe according to an embodiment of the present invention includes a step of immersing the austenitic stainless steel pipe for 30 to 120 seconds in a mixed acid solution of nitric acid and hydrofluoric acid at a temperature of 40 to 60°C. In the mixed acid solution, 10 to 20 vol% of nitric acid and 6 to 8 vol% of hydrofluoric acid are mixed.

Description

오스테나이트계 스테인리스강 파이프의 산세방법 {PICKLING METHOD OF AUSTENITIC STAINLESS PIPE}Pickling method of austenitic stainless steel pipes {PICKLING METHOD OF AUSTENITIC STAINLESS PIPE}

본 발명은 오스테나이트계 스테인리스강 파이프의 내식성을 향상시키는 산세기술에 관한 것이다.The present invention relates to a pickling technique that improves the corrosion resistance of austenitic stainless steel pipes.

일반적으로 스테인리스강은 그 표면에 크롬이 농화된 두께 10nm이하의 얇은 산화 피막이 존재하여 고유의 내식성을 가지게 된다. 이러한 산화 피막은 스테인리스강이 대기상태에 있거나 물속에 있을 때 자연적으로 생성되어, 산소, 수분, 염분 등 외부환경의 산화물질로부터 금속을 보호하여 산화반응을 억제하게 된다.In general, stainless steel has an inherent corrosion resistance because a thin oxide film having a thickness of 10 nm or less is concentrated on the surface of chromium. Such an oxide film is naturally generated when stainless steel is in the air or in water, thereby protecting metals from oxides of the external environment such as oxygen, moisture, and salt, thereby suppressing oxidation reactions.

이러한 산화 피막의 성분은 주로 크롬계 산화물이며, 철계 산화물과 혼재하여 표면에 존재하는데, 피막 중의 성분이 변할 경우 스테인리스강의 내식성이 개선되기도 하고 나빠지기도 한다. The components of the oxide film are mainly chromium oxides, and are present on the surface in a mixture with iron oxides. When the components in the film change, the corrosion resistance of stainless steel may improve or deteriorate.

일반적으로 스테인리스강 파이프를 조관 후에 산세할 때 산세용액의 조성에 따라서 파이프 표면의 불순물 제거능과 부동태피막성능이 변화하고 내식성이 영향을 크게 받게 된다.In general, when pickling a stainless steel pipe after pipe preparation, the ability to remove impurities and passivation of the surface of the pipe varies depending on the composition of the pickling solution, and corrosion resistance is greatly affected.

본 발명은 오스테나이트계 스테인리스강 파이프의 산세처리를 위한 불산농도를 최적화함으로써 내식성이 우수한 오스테나이트계 스테인리스강 파이프의 산세방법을 제공한다.The present invention provides a method of pickling an austenitic stainless steel pipe having excellent corrosion resistance by optimizing the hydrofluoric acid concentration for pickling the austenitic stainless steel pipe.

본 발명의 일 실시예에 따른 오스테나이트계 스테인리스강 파이프를 산세하는 방법은, 40~60℃온도의, 질산 및 불산이 혼합된 혼산액에 30~120초간 상기 오스테나이트계 스테인리스강 파이프를 침지하는 것;을 포함하고, 상기 혼산액은 10~20 vol.%의 질산과 6~8 vol.%의 불산이 혼합된 것을 특징으로 한다.Method of pickling austenitic stainless steel pipe according to an embodiment of the present invention, to immerse the austenitic stainless steel pipe for 30 to 120 seconds in a mixed solution of nitric acid and hydrofluoric acid at a temperature of 40 ~ 60 ℃ It includes; and the mixed solution is characterized in that 10 to 20 vol.% of nitric acid and 6 to 8 vol.% of hydrofluoric acid are mixed.

또한, 상기 오스테나이트계 스테인리스강은 중량%로, Cr:15~25%, Ni:7~20%, Si: 3.0% 이하, Mn: 15.0% 이하, Nb: 0.7% 이하, Ti: 0.5% 이하, Al: 5.0% 이하, C: 0.5% 이하, N: 2.0% 이하, Mo: 5.0% 이하, 잔부 Fe 및 불가피한 불순물을 포함할 수 있다.In addition, the austenitic stainless steel is in weight percent, Cr:15 to 25%, Ni: 7 to 20%, Si: 3.0% or less, Mn: 15.0% or less, Nb: 0.7% or less, Ti: 0.5% or less , Al: 5.0% or less, C: 0.5% or less, N: 2.0% or less, Mo: 5.0% or less, balance Fe and unavoidable impurities.

본 발명에 따르면, 오스테나이트계 스테인리스강 파이프 표면의 오염물을 효과적으로 제거하고 부동태피막을 강화함으로써 스테인리스강의 내식성을 향상시킬 수 있다.According to the present invention, corrosion resistance of stainless steel can be improved by effectively removing contaminants on the surface of austenitic stainless steel pipe and strengthening the passivation film.

또한, 본 발명에 따른 산세기술을 적용함으로써 건자재 파이프와 같은 대기환경 하에 있는 오스테나이트계 스테인리스강 파이프의 부식반응을 억제하고 내식성을 효과적으로 개선할 수 있다.In addition, by applying the pickling technology according to the present invention, it is possible to suppress the corrosion reaction of the austenitic stainless steel pipe under an atmospheric environment such as a construction material pipe and effectively improve corrosion resistance.

도 1은 일 실시예에 따른 오스테나이트계 스테인리스강 파이프의 표면 내식성을 KS기준으로 공식전위를 측정한 결과이다.
도 2는 비교예에 따른 오스테나이트계 스테인리스강 파이프의 표면 내식성을 KS기준으로 공식전위를 측정한 결과이다.1 is a result of measuring the official potential of the surface corrosion resistance of the austenitic stainless steel pipe according to an embodiment based on KS.
2 is a result of measuring the official potential of the surface corrosion resistance of the austenitic stainless steel pipe according to the comparative example based on KS.

이하에서는 본 발명의 실시예를 상세히 설명한다. 이하의 실시예는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 본 발명의 사상을 충분히 전달하기 위해 제시하는 것이다. 본 발명은 여기서 제시한 실시예만으로 한정되지 않고 다른 형태로 구체화될 수도 있다. 또한 어떤 부분이 어떤 구성요소를 "포함"한다고 할 때, 이는 특별히 반대되는 기재가 없는 한 다른 구성요소를 제외하는 것이 아니라 다른 구성요소를 더 포함할 수 있는 것을 의미한다. 단수의 표현은 문맥상 명백하게 예외가 있지 않는 한, 복수의 표현을 포함한다.Hereinafter, embodiments of the present invention will be described in detail. The following examples are presented to sufficiently convey the spirit of the present invention to those of ordinary skill in the art. The present invention is not limited to only the examples presented herein, but may be embodied in other forms. Also, when a part “includes” a certain component, this means that other components may be further included, rather than excluding other components, unless otherwise specified. Singular expressions include plural expressions, unless the context clearly has an exception.

본 발명의 오스테나이트계 스테인리스강 파이프의 산세방법은, 오스테나이트계 스테인리스강 파이프를 40~60℃의 온도범위 및 10~20 vol.%의 질산용액과 6~8 vol.%의 불산 혼합용액에서 30~120초간 침지함으로써 파이프 표면의 오염물을 제거하고 부동태피막성능을 개선하는 것을 특징으로 한다.The method of pickling the austenitic stainless steel pipe of the present invention, the austenitic stainless steel pipe in a temperature range of 40 ~ 60 ℃ and 10 ~ 20 vol.% of nitric acid solution and 6 ~ 8 vol.% of hydrofluoric acid mixed solution It is characterized by removing contaminants from the pipe surface and improving passivation performance by immersion for 30 to 120 seconds.

본 발명은 오스테나이트계 스테인리스강 파이프의 산세방법에 관한 것으로, 그 대상이 특정한 오스테나이트계 스테인리스강의 조성성분에 제한되지 않으며 다양한 조성성분을 갖는 오스테나이트계 스테인리스강에 적용 가능하다.The present invention relates to a method for pickling an austenitic stainless steel pipe, the object of which is not limited to the compositional component of a specific austenitic stainless steel and is applicable to austenitic stainless steel having various compositional components.

그 일예로, 상기 오스테나이트계 스테인리스강은 중량%로, Cr:15~25%, Ni:7~20%, Si: 3.0% 이하, Mn: 15.0% 이하, Nb: 0.7% 이하, Ti: 0.5% 이하, Al: 5.0% 이하, C: 0.5% 이하, N: 2.0% 이하, Mo: 5.0% 이하, 잔부 Fe 및 불가피한 불순물을 포함할 수 있다.As an example, the austenitic stainless steel is in weight percent, Cr:15 to 25%, Ni: 7 to 20%, Si: 3.0% or less, Mn: 15.0% or less, Nb: 0.7% or less, Ti: 0.5 % Or less, Al: 5.0% or less, C: 0.5% or less, N: 2.0% or less, Mo: 5.0% or less, balance Fe and unavoidable impurities.

개시된 실시예에 따른 오스테나이트계 스테인리스강 파이프의 산세방법은 40~60℃의 온도범위 및 10~20 vol.%의 질산용액과 6~8 vol.%의 불산 혼합용액에서 30~120초간 오스테나이트계 스테인리스강 파이프를 침지함으로써 파이프 표면의 오염물을 제거하고 부동태피막성능을 개선시킬 수 있다.The method of pickling the austenitic stainless steel pipe according to the disclosed embodiment is austenite for 30 to 120 seconds in a temperature range of 40 to 60°C and a 10 to 20 vol.% nitric acid solution and a 6 to 8 vol.% hydrofluoric acid mixed solution. By immersing the stainless steel pipe, it is possible to remove contaminants from the pipe surface and improve passivation performance.

개시된 실시예에 따른 산세방법에서 산세온도가 40℃ 미만이면 충분한 오염물 제거가 힘들고, 60℃를 초과하면 유해가스인 NOx가 다량 발생되므로, 산세온도는 40~60℃로 제한될 수 있다.In the pickling method according to the disclosed embodiment, if the pickling temperature is less than 40°C, it is difficult to remove sufficient pollutants, and if it exceeds 60°C, a large amount of NOx, a harmful gas, is generated, so the pickling temperature may be limited to 40 to 60°C.

또한 용액내의 불산 농도가 6 vol% 이상에서 철계산화물과 같은 불순물과 오염물이 활발히 제거되나, 8 vol% 초과하는 불산농도에서는 스테인리스강 모재가 침식되는 문제가 발생되므로, 불산의 농도는 6~8 vol%로 제한된다.In addition, impurities and contaminants such as iron-based oxides are actively removed when the concentration of hydrofluoric acid in the solution is 6 vol% or more, but when the concentration of hydrofluoric acid exceeds 8 vol%, the problem of erosion of the stainless steel base material occurs, the concentration of hydrofluoric acid is 6~8 It is limited to vol%.

또한, 개시된 실시예에 따른 산세방법은 산세처리시간을 30~120초의 범위로 유지할 경우, 불순물의 제거가 최적화될 수 있다. 만일 30초 미만으로 처리할 경우에는 불순물 제거 시간이 불충분하며, 120초를 초과하여 처리할 경우에는 스테인리스강 모재가 침식될 수 있다.In addition, in the pickling method according to the disclosed embodiment, when the pickling treatment time is maintained in a range of 30 to 120 seconds, removal of impurities may be optimized. If the treatment is performed for less than 30 seconds, the impurity removal time is insufficient, and when the treatment is performed for more than 120 seconds, the stainless steel base material may be eroded.

이하, 실시예를 통하여 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.

(실시예)(Example)

크롬함유량이 18중량%이고 니켈함량이 8중량%이고 두께가 1.0mm이고 직경이 30mm인 스테인리스강 파이프를 마련하였다. 이렇게 마련된 스테인리스강 파이프를 전술한 산세방법에 따라, 온도 50도의 질산 15vol%와 불산 6%vol농도의 혼합용액에서 60초간 처리하여 파이프표면의 불순물과 오염을 제거하였다.A stainless steel pipe having a chromium content of 18% by weight, a nickel content of 8% by weight, a thickness of 1.0mm, and a diameter of 30mm was prepared. The stainless steel pipe thus prepared was treated in a mixed solution of 15 vol% of nitric acid and 6 vol of hydrofluoric acid at a temperature of 50 degrees for 60 seconds at a temperature of 50 degrees to remove impurities and contamination on the pipe surface.

그리고 비교예는 오스테나이트계 스테인리스강 파이프를 온도 50도의 질산 15%와 불산 3%농도의 혼합용액에서 60초간 처리하였다. And in the comparative example, the austenitic stainless steel pipe was treated for 60 seconds in a mixed solution of 15% nitric acid and 3% hydrofluoric acid at a temperature of 50 degrees.

이후, 전술한 본 발명의 실시예에 따라 산세처리를 실시한 스테인리스강 파이프와 비교예에 따라 산세처리한 스테인리스강 파이프에 대하여 KS D 0238 기준으로 공식전위를 측정하여 내식성을 비교하였고 그 결과를 도 1 및 도 2에 나타내었다. Subsequently, the corrosion resistance was compared by measuring the official potential based on KS D 0238 for the stainless steel pipe subjected to the pickling treatment according to the embodiment of the present invention and the stainless steel pipe subjected to the pickling treatment according to the comparative example. And shown in FIG. 2.

도 1은 본 발명의 실시예에 따른 산세방법에 따라 산세처리한 오스테나이트계 스테인리스강 파이프 표면을 KS기준으로 공식전위를 측정한 결과이다. 그래프의 x축은 부식반응 속도인 전류값이고 y축은 금속에 인가된 전위값으로서, 전류값이 10~100㎂/cm2을 초과할 때의 전위값을 측정하여 공식전위라고 칭하고 그 값이 높을수록 내식성이 우수하다고 판정한다.1 is a result of measuring the official potential of the austenitic stainless steel pipe surface subjected to pickling according to the pickling method according to an embodiment of the present invention based on KS. As with the x-axis represents reaction rate of the corrosion current value of the graph is the y axis is applied to the metal potential value, referred as formula potential by measuring the potential values at the time of the current value exceeds 10 ~ 100㎂ / cm 2 The higher the value It is judged that the corrosion resistance is excellent.

도 1에 도시된 것처럼, 본 발명의 실시예에 따른 산세방법에 따라 산세처리한 오스테나이트계 스테인리스강 파이프의 공식전위는 391mV로 높게 측정되었다.As shown in Figure 1, the official potential of the austenitic stainless steel pipe pickled according to the pickling method according to an embodiment of the present invention was measured to be high at 391 mV.

도 2는 비교예에 따른 산세방법에 따라 산세처리한 오스테나이트계 스테인리스강 파이프 표면을 KS기준으로 공식전위를 측정한 결과이다. 그래프의 x축은 부식반응 속도인 전류값이고 y축은 금속에 인가된 전위값으로서, 전류값이 10~100㎂/cm2을 초과할때의 전위값을 측정하여 공식전위라고 칭하고 그 값이 높을수록 내식성이 우수하다고 판정한다. 비교예에 따른 산세방법에 따라 산세처리된 오스테나이트계 스테인리스강 파이프의 공식전위는 108mV로 실시예에 비해 낮게 측정되었다.2 is a result of measuring the official potential of the surface of the austenitic stainless steel pipe pickled according to the pickling method according to the comparative example based on KS. In the graph, the x-axis is the current value that is the corrosion reaction rate, and the y-axis is the potential value applied to the metal. When the current value exceeds 10 to 100 ㎂/cm 2 , the potential value is measured and called the official potential. It is judged that the corrosion resistance is excellent. The official potential of the austenitic stainless steel pipe pickled according to the pickling method according to the comparative example was 108 mV, which was lower than in the example.

도 1 및 도 2에 나타난 바와 같이, 본 발명의 실시예에 따라 산세처리된 오스테나이트계 스테인리스강 파이프의 공식전위가 비교예에 따라 산세처리된 오스테나이트계 스테인리스강 파이프의 공식전위보다 231mV 높게 측정되어 내식성이 우수함을 알 수 있다.As shown in Figures 1 and 2, the official potential of the austenitic stainless steel pipe pickled according to an embodiment of the present invention is measured 231 mV higher than the official potential of the austenitic stainless steel pipe pickled according to a comparative example It can be seen that the corrosion resistance is excellent.

상술한 바에 있어서, 본 발명의 예시적인 실시예들을 설명하였지만, 본 발명은 이에 한정되지 않으며 해당 기술 분야에서 통상의 지식을 가진 자라면 다음에 기재하는 특허청구범위의 개념과 범위를 벗어나지 않는 범위 내에서 다양한 변경 및 변형이 가능함을 이해할 수 있을 것이다.As described above, although exemplary embodiments of the present invention have been described, the present invention is not limited thereto, and a person having ordinary skill in the art does not depart from the concept and scope of the following claims. It will be understood that various modifications and variations are possible.

Claims (2)

오스테나이트계 스테인리스강 파이프를 산세하는 방법에 있어서,
40~60℃온도의, 질산 및 불산이 혼합된 혼산액에 30~120초간 상기 오스테나이트계 스테인리스강 파이프를 침지하는 것;을 포함하고,
상기 혼산액은 10~20 vol.%의 질산과 6~8 vol.%의 불산이 혼합된 오스테나이트계 스테인리스강 파이프의 산세방법.In the method of pickling austenitic stainless steel pipe,
It includes; immersing the austenitic stainless steel pipe for 30 to 120 seconds in a mixed acid mixture of nitric acid and hydrofluoric acid at a temperature of 40 to 60°C;
The mixed solution is a pickling method of an austenitic stainless steel pipe in which 10-20 vol.% nitric acid and 6-8 vol.% hydrofluoric acid are mixed. 제1항에 있어서,
상기 오스테나이트계 스테인리스강은 중량%로, Cr:15~25%, Ni:7~20%, Si: 3.0% 이하, Mn: 15.0% 이하, Nb: 0.7% 이하, Ti: 0.5% 이하, Al: 5.0% 이하, C: 0.5% 이하, N: 2.0% 이하, Mo: 5.0% 이하, 잔부 Fe 및 불가피한 불순물을 포함하는 오스테나이트계 스테인리스강 파이프의 산세방법.According to claim 1,
The austenitic stainless steel is in weight%, Cr: 15-25%, Ni: 7-20%, Si: 3.0% or less, Mn: 15.0% or less, Nb: 0.7% or less, Ti: 0.5% or less, Al : 5.0% or less, C: 0.5% or less, N: 2.0% or less, Mo: 5.0% or less, pickling method of austenitic stainless steel pipe containing residual Fe and unavoidable impurities.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114214631A (en) * 2021-12-20 2022-03-22 太原科技大学 Acid pickling process of austenitic iron-nickel-based alloy welded pipe

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114214631A (en) * 2021-12-20 2022-03-22 太原科技大学 Acid pickling process of austenitic iron-nickel-based alloy welded pipe

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