KR900007452B1 - Ni alloy for corrision resistant - Google Patents
Ni alloy for corrision resistant Download PDFInfo
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Abstract
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Description
제1도는 1000。K, Ar, 20% O2,2% Cl2혼합가스내에서 합금의 부식반응결과를 나타내는 그라프.FIG. 1 is a graph showing the results of corrosion reactions of alloys in 1000 ° K, Ar, 20%
제2도는 1100。K, Ar, 20% O2, 2.8% Cl2혼합가스내에서 합금의 부식 반응결과를 나타내는 그라프.FIG. 2 is a graph showing the results of corrosion reactions of alloys in a mixture of 1100 ° K, Ar, 20% O 2 , and 2.8% Cl 2 .
제3도는 1200。K, Ar, 20% O2,1% Cl2혼합가스내에서 합금의 부식반응결과릍 나타내는 그라프.3 is a graph showing the results of corrosion reactions of alloys in 1200 ° K, Ar, 20% O 2 and 1% Cl 2 mixed gases.
제4도는 1200。K, Ar, 20% O2,2.8% Cl2혼합가스내에서 합금의 부식반응결과를 나타내는 그라프.4 is a graph showing the results of corrosion reaction of alloys in 1200 ° K, Ar, 20% O 2, 2.8% Cl 2 mixed gas.
제5도는 1200。K, Ar, 600ppm Cl2혼합가스내에서의 내부산화도를 나타내는 사진.5 is a photograph showing the internal oxidation degree in 1200 ° K, Ar, 600ppm Cl 2 mixed gas.
제6도는 보호피막처리후 900℃, Ar, 20%, O2, 1% Cl2혼합가스내에서 합금의 부식반응결과를 나타내는 그라프이다.6 is a graph showing the results of corrosion reaction of the alloy in 900 ℃, Ar, 20%, O 2 , 1% Cl 2 mixed gas after the protective coating treatment.
본 발명은 염소가스를 함유한 고온의 산화분위기에서도 내식성이 뛰어난 고온 초내식성 Ni계 합금에 관한 것이다.The present invention relates to a high temperature super corrosion resistant Ni-based alloy excellent in corrosion resistance even in a high temperature oxidation atmosphere containing chlorine gas.
고온에서 염소가스 발생에 의한 부식이 심각하게 문제가 되는 산업공정 또는 부식부위로는, 폴리비닐 클로라이드(PVC)성분이 함유된 제품의 소각공정, 폐유의 정련공정, 저질탐을 사용하는 산업공정, 젯트엔진의 가스터빈부위, 알루미늄 제련의 탈가스공정시 염소가스를 플럭스(Flux)로 사용하는 알루미늄 재용해로의 열교환기 부위등이 있다. 종래의 공지기술중 고온에서 염소가스에 의한 부식에 관하여 연구된 기술 및 합금은 없으나 일반적 내식성 및 고온산화성이 우수한 소재로는 AISI 304 스테인레스강에 몰리부데늄(Mo)을 첨가한 AISI 316계 스테인레스강 및 크롬산화 피막을 형성하는 니켈계 특수합금인 인코넬(Inconel) 600등이 있다.Industrial processes or corrosion areas where corrosion by chlorine gas generation is a serious problem at high temperatures include incineration of products containing polyvinyl chloride (PVC), refining of waste oil, industrial processes using low quality probes, The gas turbine part of the jet engine, the heat exchanger part of the aluminum remelting furnace which uses chlorine gas as a flux in the degassing process of aluminum smelting, etc. are mentioned. Although there are no techniques and alloys studied for corrosion by chlorine gas at a high temperature in the prior art, general AISI 316 stainless steels added with molybdenum (Mo) to AISI 304 stainless steel have excellent corrosion resistance and high temperature oxidation resistance. And Inconel 600, which is a nickel-based special alloy forming a chromium oxide film.
그러나 이들 내식강들은 고온의 염소가스분위기에서는 금속과 염소간 화합물을 형성시키므로 이들 염화물의 낮은 용융점과 높은 기화 압력때문에 고온내식성은 극히 취약해지는 결점이 있다.However, these corrosion resistant steels form compounds between metals and chlorine in a high temperature chlorine gas atmosphere, so the low temperature melting point and high vaporization pressure of these chlorides make the corrosion resistance extremely weak.
종래 고온 내식성 소재들은 일반적으로 크롬을 다량 첨가하여 크롬피막형성에 의한 내식성향상을 꾀한 것이다.Conventional high temperature corrosion resistant materials are generally intended to improve the corrosion resistance by forming a large amount of chromium coating.
그러나. 크롬 피막은 고온에서 염소가스의 농도가 높아질수록 쉽게 파괴되어 기지 금속인 니켈과 염소가스의 직접적인 반응을 제어하지 못하는 결점이 있다.But. The chromium film is easily destroyed as the concentration of chlorine gas increases at high temperatures, and thus there is a drawback that the chromium film cannot control the direct reaction of nickel with chlorine gas.
또한, 특정 온도에서는 크롬의 함량이 증가할수록 합금 표면에서 산소의 활동도를 낮추며 상대적으로 염소가스의 활동도를 향상시켜 오히려 부식속도를 촉진하기도 한다.In addition, at a certain temperature, as the content of chromium increases, the activity of oxygen on the surface of the alloy is lowered, and the activity of chlorine gas is relatively improved, and thus the corrosion rate is accelerated.
본 발명의 목적은 종래 내식용 강의 문제점을 해결하기 위한 것으로서, 염소-산소혼합 가스에 의한 고온부식저항을 크게 향상시킨 고온 초내식용 니켈계 특수합금을 제공하기 위한 것이다.An object of the present invention is to solve the problems of conventional corrosion-resistant steel, to provide a high-temperature super corrosion-resistant nickel-based special alloy that greatly improved the high temperature corrosion resistance by chlorine-oxygen mixed gas.
고 크롬 첨가강의 다른 문제점으로서 세계 크롬 매장량의 90% 이상을 적성국가에서 점유하고 있어 향후크롬 금속이 전략 원소로 사용될 가능성을 배제할수 없다.Another problem with high chromium-added steels is that more than 90% of the world's chromium reserves are in the host country, so the possibility of future use of chromium metal as a strategic element cannot be ruled out.
본 발명의 다른 목적은 고온 초 내식용 합금 설계에 있어서 자유세계의 희귀 부존, 자원인 크롬의 첨가량을 극소화하여 미래에 크롬 금속이 전략원소로 이용될 경우에 대비하기 위한 것이다.Another object of the present invention is to minimize the amount of chromium, which is rare in the free world and resource in the design of high temperature super corrosion resistant alloys, to prepare for the case where chromium metal is used as a strategic element in the future.
본 발명강인 고온 초 내식용 특수합금은 기존의 고온내식용 소재와는 달리 크롬의 첨가량을 극소화 하였으며 그 대체 원소로 알루미늄을 첨가한 것이다.The high temperature super corrosion resistant special alloy of the present invention, unlike the existing high temperature corrosion resistant material, minimized the amount of chromium added and added aluminum as an alternative element.
크롬과 알루미늄 첨가의 효과 및 한계를 설정하기 위하여 크롬과 알루미늄을 동시에 첨가하지 않은 니켈-크롬 및 니켈-알루미늄 이원계 합금을 크롬과 알루미늄을 동시에 첨가한 본 발명강과 함께 통상적인 주조 방법으로 주조하여 열처리공정을 거친 후 각기 특성을 비교하였으며 기존 니켈계 합금인 인코넬(Inconel) 600와 Hastelloy S와의 특성도 비교 분석하였다.In order to set the effects and limitations of chromium and aluminum addition, nickel-chromium and nickel-aluminum binary alloys without chromium and aluminum are simultaneously cast together with the present invention steel with chromium and aluminum, followed by a conventional casting method for heat treatment. After comparison, the characteristics were compared with those of Inconel 600 and Hastelloy S.
본 발명강의 특성을 비교 분석하기 위한 소재들의 조성은 표 1과 같다.The composition of the materials for comparatively analyzing the characteristics of the inventive steel is shown in Table 1.
[표 1]TABLE 1
고온 내식성의 평가 방법으로는 열중량 분석법(Thermogravimetric Analysis)이 이용되었다.Thermogravimetric Analysis was used to evaluate high temperature corrosion resistance.
열중량 분석법은 고온에서 합금과 기체가 반응할때 생성되는 합금 질량의 증,감을 시간의 함수로 연속적으로 기록하여 부식의 속도를 측정하는 방법이다.Thermogravimetric analysis is a method of measuring the rate of corrosion by continuously recording the increase and decrease of the mass of an alloy as a function of time when the alloy and gas react at high temperatures.
이하 본 발명강의 특성을 실시예에 의거 상세히 설명한다.Hereinafter, the characteristics of the inventive steel will be described in detail with reference to Examples.
실시예 1Example 1
Ni-Cr, Ni-Al 이온계 합금(A5,C5,C15 및 C30)과 발명강을(1,2,3)을 l00°K에서 Ar,20% O2,2% Cl2혼합가스와 150분간 반응시켰다.Ni-Cr, Ni-Al ionic alloys (A5, C5, C15 and C30) and inventive steels (1,2,3) were mixed with Ar, 20%
제1도에 나타난 바와같이 합금 A5와 발명강은 우수한 내식성을 보여주고 있는 반면 고크롬 첨가강인 합금 C30는 가장 빠른 부식속도를 보여주고 있다. 여기서 발명강 1,2,3(이하, 실시예에서는 "발명강"이라 칭함) 모두 거의 유사한 값을 나타내었기 때문에 발명강으로 총칭하여 나타내었다.As shown in FIG. 1, alloy A5 and the inventive steel showed excellent corrosion resistance, while alloy C30, a high chromium-added steel, showed the fastest corrosion rate. Herein, the
크롬 첨가량의 증가가 부식 속도를 증가시키는 이유는 전술한 바와같이 합금 표면에서의 산소의 활동도와 관계가 있다.The reason why the increase in the amount of chromium increases the corrosion rate is related to the activity of oxygen on the alloy surface as described above.
이 실험 결과는 1000°K 염소-산소 혼합가스 분위기에서 크롬 산화피막이 형성됨으로 인하여 내식성 향상에 오히려 어려움이 있음을 보여주고 있다.The test results show that the chromium oxide film is formed in a 1000 ° K chlorine-oxygen mixed gas atmosphere, which makes it difficult to improve corrosion resistance.
반면 알루미늄 첨가에 의해 형성된 피막은 염소가스의 침투를 방지하여 기지 금속인 니켈과 염소가스간의 직접적인 반응을 억제하여 내식성을 월등히 향상시키고 있다.On the other hand, the film formed by the addition of aluminum prevents the penetration of chlorine gas, thereby suppressing the direct reaction between nickel and chlorine gas, which is greatly improved in corrosion resistance.
실시예 2Example 2
Ni-Cr, Ni-Al 이원계 합금(A5,C5,C15 및 C30)과 발명강을 1100°K에서 Ar,20% O2,2.8% Cl2혼합가스와 150분간 반응시켰다.Ni-Cr, Ni-Al binary alloys (A5, C5, C15 and C30) and the inventive steel were reacted with Ar, 20% O 2 , 2.8% Cl 2 mixed gas for 150 minutes at 1100 ° K.
제2도에서 보여지는 것과같이 발명강만이 극히 우수한 내식성을 보여주고 있다. 실시예 1의 경우와는 달리 크롬의 첨가량이 증가할수록 내식성은 향상되고 있으나 크롬피막형성에 의한 고온 내식성의 향상은 역시 기대하기 어려웠다. .As shown in FIG. 2, only the inventive steel shows extremely excellent corrosion resistance. Unlike the case of Example 1, as the amount of chromium is increased, the corrosion resistance is improved, but the improvement of the high temperature corrosion resistance by chromium film formation is also difficult to expect. .
알루미늄을 단독으로 첨가할 경우의 내식성 역시 알루미늄과 크롬을 동시에 첨가할 경우에 비하여 극히 떨어졌다.Corrosion resistance when aluminum is added alone is also significantly lower than when aluminum and chromium are added simultaneously.
실시예 1의 결과와 비교할때 온도상승에 따라 부식속도는 급속히 증가하여 이는 니켈 클로라이드(NiCl2)기화 압력의 급속한 증가에 기인되는 것이다.Compared with the results of Example 1, the corrosion rate increases rapidly with temperature rise, which is due to the rapid increase in the nickel chloride (NiCl 2 ) vaporization pressure.
실시예 3Example 3
본 발명강과 기존 니켈계 내식용 강인 인코넬 600와의 내식성을 비교분석할 목적으로 1200°K Ar, 20% O2, 1% Cl2혼합가스내에서 실험을 행하였다.In order to analyze the corrosion resistance between the inventive steel and the conventional nickel-based corrosion resistant steel, Inconel 600, an experiment was conducted in 1200 ° K Ar, 20% O 2 , and 1% Cl 2 mixed gas.
제3도에서 보여지는 바와같이 알루미늄이 첨가된 합금이 크롬 첨가 합금에 비하여 월등히 우수한 내식성을 보여주고 있다.As shown in FIG. 3, the aluminum-added alloy shows excellent corrosion resistance compared to the chromium-added alloy.
고크롬 첨가강인 합금 C30의 부식속도는 시간이 경과할수록 급속히 증가하고 있으며 이는 염소가스에의한 크롬 피막의 파괴에 기인한다.The corrosion rate of alloy C30, a high chromium-added steel, increases rapidly with time, which is due to the destruction of the chromium film by chlorine gas.
실시예 4Example 4
시간 경과에 다른 부식속도 증감의 효과를 관측하기 위하여 부식 분위기 내의 염소가스의 함량을 2.8%로 상승시켜 합금의 내식성을 평가하였다.In order to observe the effect of different corrosion rate increase and decrease over time, the corrosion resistance of the alloy was evaluated by increasing the content of chlorine gas in the corrosion atmosphere to 2.8%.
제4도에서 보여지는 바와같이 l200°K Ar, 20% O2, 2.8% Cl2. 분위기에서는 본 발명강을 제외한 모든 합금은 내식성을 거의 상실하고 있다.As shown in FIG. 4, l200 ° K Ar, 20% O 2 , 2.8% Cl 2 . In the atmosphere, all alloys except the inventive steel almost lose corrosion resistance.
참고로, 부식속도를 단위 면적, 단위시간당 합금의 무게감소의 함수로 측정할때 대표적 합금의 무게 감소의 값은 표2와 같다.For reference, when the corrosion rate is measured as a function of the unit area and the weight loss of the alloy per unit time, the weight loss values of the typical alloys are shown in Table 2.
[표 2]TABLE 2
표 2에서 보여지는 바와같이 본 발명강은 본 실시예중 가장 심한 부식 분위기에서도 극히 우수한 내식성을 보여주고 있다.As shown in Table 2, the inventive steel shows extremely excellent corrosion resistance even in the most severe corrosive atmosphere of this example.
실시예 5Example 5
합금 A5는 연소가스의 농도가 낮은 경우 발명강과 더불어 고온에서도 극히 우수한 내식성을 보여주고 있다.Alloy A5 shows extremely good corrosion resistance even at high temperatures in addition to the inventive steel at low combustion gas concentrations.
니켈-알루미늄 이원계 합금에서 크롬첨가의 영향을 조사하기 위하여 합금A5와 발명강(l)을 1200。K에서 Ar, 600ppm Cl2혼합가스와 반응시킨후단면을 절단하여 내부(Internal) 부식성을 조사하였다.In order to investigate the effect of chromium addition on nickel-aluminum binary alloys, internal corrosion was investigated by reacting Alloy A5 and Invented Steel (l) with Ar, 600ppm Cl 2 mixed gas at 1200 ° K. .
제5도에서 보여지는 바와같이 크롬이 함유되지 않은 합금 A5는 혼합가스내에 불순물로 존재하는 약 100ppm의 산소와 반응하여 심각한 내부부식 현상을 보여주는 반면 본 발명강(1)은 산소의 침투를 억제하여 내부부식 현상을 보여 주지 않고 있다.As shown in FIG. 5, alloy A5, which does not contain chromium, reacts with about 100 ppm of oxygen present as impurities in the mixed gas to show severe corrosion resistance, whereas the inventive steel (1) suppresses the penetration of oxygen. It does not show internal corrosion.
실시예 6Example 6
위 기술한 실시예들과는 달리 인위적인 산화피막형성이 내식성에 미치는 영향을 조사하기 위하여 인코넬 600, Hastelloy S와 본 발명강을 900℃에서 순수 산소와 24시간 동안 반응시켜 보호피막을 형성시킨후, 온도 변화없이 Ar, 50% O2. 1% Cl2혼합가스와 24시간동안 반응시켰다.Unlike the above-described embodiments, in order to investigate the effect of artificial oxide film formation on the corrosion resistance, Inconel 600, Hastelloy S and the inventive steel were reacted with pure oxygen at 900 ° C. for 24 hours to form a protective film, followed by temperature change. Without Ar, 50% O 2 . The mixture was reacted with 1% Cl 2 mixed gas for 24 hours.
제6도에서 보여지는 바와같이 크롬보호 피막처리된 기존 니켈계 강은 내식성을 완전 상실하는 반면 본 발명강은 장시간의 반응에도 불구하고 극히 우수한 내식성을 보여주고 있다.As shown in FIG. 6, the existing nickel-based steel coated with chromium protection completely loses corrosion resistance, whereas the present invention steel shows extremely excellent corrosion resistance despite a long time reaction.
위 실시예들에서 보여지는 바와같이 본 발명강은 염소가스가 함유된 고온의 부식분위기에서 기존 내식용강인 인코넬 600등에 비교할때 월등히 우수한 고온 초 내식용 강임을 입증하고 있다.As shown in the above examples, the present invention has proved to be an excellent high temperature super corrosion resistant steel in comparison with the conventional corrosion resistant steel, Inconel 600, in a high temperature corrosion atmosphere containing chlorine gas.
본 발명에 대한 상기 실시예의 결과 및 합금의 상태도를 고려할때, Ni 금속에 대한 알루미늄(Al), 크롬(Cr) 그리고 불순물 첨가량의 한계는 다음과 같음을 알수 있다.Considering the results of the above embodiment and the state diagram of the alloy, it can be seen that the limits of the addition amount of aluminum (Al), chromium (Cr) and impurities to Ni metal are as follows.
본 발명에서 Cr과 Al을 동시 첨가하는 이유는 Al단독 첨가에 비하여 Cr과 A1을 동시에 첨가하는 경우에 알루미나 보호피막 아래에 크로미아 피막을 형성함으로서 보호 피막의 두께 및 접착력을 증가시켜 산소의 침투를 방지할수 있기 때문이다.The reason why simultaneous addition of Cr and Al in the present invention is to increase the thickness and adhesion of the protective film by increasing the thickness and adhesion of the protective film by forming a chromia film under the alumina protective film when simultaneously adding Cr and A1 as compared to Al alone. Because it can prevent.
Ni 금속에 대한 A1의 고용량은 온도에 따라 약간씩 차이는 있으나 상기 실시예의 온도 구간에서는 5%이하로 제한함이 효과적이다.The high capacity of A1 for Ni metal is slightly different depending on the temperature, but it is effective to limit it to 5% or less in the temperature section of the embodiment.
한편, Al 첨가량이 이를 초과할 때에는 Ni3Al 형태의 금속간 화합물을 형성케되어 가공성을 극히 저하시키는 폐단이 노출된다. 또한 Al 첨가량이 2% 이하인 경우에는 내부의 선택산화를 동반하게 되기때문에 Al 첨가범위를 2-5wt%로 하였다.On the other hand, when the amount of Al added exceeds this, a closed end is formed that forms an intermetallic compound in the form of Ni 3 Al, thereby extremely reducing workability. In addition, when the amount of Al added was 2% or less, the addition of Al was carried out, so that the amount of Al added was 2-5 wt%.
Cr의 첨가량은 20% 정도까지 아무런 제한을 받지 않으나, Cr을 5%이상 첨가하면 고온에서 Al을 함유한 피막형성 대신에 Cr을 함유한 피막을 형성케되어 오히려 부식을 조장할수가 있다.The amount of Cr added is not limited to about 20%, but when Cr is added 5% or more, a film containing Cr is formed instead of Al-containing film at a high temperature, which may promote corrosion.
또한 Cr을 3% 이하 첨가하면 금속내부에서의 산화층 형성이 어려워지게 되며, 내부의 선택산화를 수반하기 때문에 Cr 첨가 범위를 3-5wt%로 하였다.In addition, when 3% or less of Cr is added, it becomes difficult to form an oxide layer in the metal, and the Cr addition range is set to 3-5wt% because it involves selective oxidation inside.
Al 피막형성의 속도는 Cr 피막형성의 속도보다 훨씬 빠르므로 동량(同量)의 Al과 Cr이 첨가될때 Al 피막형성이 우선하게 된다.Since the rate of Al film formation is much faster than the rate of Cr film formation, Al film formation takes precedence when the same amount of Al and Cr are added.
본 발명의 실시예의 결과에 의하면, 5% 정도의 Cr을 첨가할때 고온에서 Al을 함유한 피막층 내부에서 NiCr2O4또는 Cr2O3상태로 크롬 산화막이 형성되었다.According to the result of the embodiment of the present invention, when adding about 5% Cr, a chromium oxide film was formed in the NiCr 2 O 4 or Cr 2 O 3 state inside the Al-containing film at high temperature.
고온 내식용 강에 있어서, 불순물의 첨가량은 극히 제한되어야 한다. 카본(C)이 첨가되면 Cr 금속과 CrxCy 형태의 화합물을 형성케 되어 Cr의 효과를 반감시키며. 황(S)의 존재는 기지금속인 Ni과 반응하여 융점이 낮은 Ni3S2화합물을 형성케되어 고온에 대한 취약성의 원인이 된다.In high temperature corrosion resistant steels, the addition amount of impurities should be extremely limited. When carbon (C) is added, Cr metal and CrxCy form compounds are formed, thereby reducing the effect of Cr. The presence of sulfur (S) reacts with Ni, a base metal, to form a Ni 3 S 2 compound having a low melting point, which is a cause of vulnerability to high temperatures.
또한 몰리부데늄(Mo)과 같이 기화압력이 높은 염화물을 형성하는 원소는 극히 제한되어야 한다.In addition, elements that form chlorides with high vapor pressure such as molybdenum (Mo) should be extremely limited.
본 발명은, 실시예의 결과와 상기의 조건들을 모두 고려하여, Ni 금속에 Cr 함량을 3-5wt% Al의 함량을 2-5wt%로하고 C의 함량을 0.01wt% 이하. S의 함량을 0.002wt% 이하로 제어하며 형성시킨 Ni계 합금으로서, 고온의 염소가스 분위기에서 Al2O3또는 NiA12O4형태의 A1을 함유한 피막형성에 의하여 고온 초 내식성 효과를 가져오는 유용한 것이다.The present invention, in consideration of both the results of the embodiment and the above conditions, the Cr content in the Ni metal to 3-5wt% Al content of 2-5wt% and C content of 0.01wt% or less. Ni-based alloy formed by controlling the content of S to 0.002wt% or less, and has a high temperature super corrosion resistance effect by forming a film containing A1 in the form of Al 2 O 3 or NiA1 2 O 4 in a high temperature chlorine gas atmosphere. It is useful.
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| KR1019870015064A KR900007452B1 (en) | 1987-12-28 | 1987-12-28 | Ni alloy for corrision resistant |
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| KR1019870015064A KR900007452B1 (en) | 1987-12-28 | 1987-12-28 | Ni alloy for corrision resistant |
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