• Clean Technology
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• v.11 no.1
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• pp.21-28
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• 2005

Nitric acid free pickling solution was applied to solve the severe environmental problems attributed to nitric acid during pickling process of stainless steel product. In points of pickling capability and erosion of stainless steel base metal, a solution contains I% of hydrochloric acid and 2% of hydrofluoric acid and hydrogen peroxide was revealed as the best alternative to conventional mixed acid of nitric acid and hydrofluoric acid. To keep the pickling capability, it was necessary to maintain the concentration ratio of hydrogen peroxide to hydrochloric acid above 0.5.

• Resources Recycling
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• v.26 no.5
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• pp.97-104
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• 2017

Nuclear fuel cladding tubes are manufactured through pilgering and the annealing process. In order to remove the oxidized layer and impurities on the surface of the tube, a pickling process is required. Zirconium (Zr) is dissolved in a HF and $HNO_3$ acid mixture during the process and the pickling waste acid, including the dissolved Zr, is completely discarded after neutralization. This study observes the effects of the residual impurities (Ba) in the pickling solution regenerated from the $BaF_2$ precipitation process on the waste pickling solution. In addition, the concentration of Ba and Zr for the actual nuclear fuel cladding tube process was optimized. The regenerated pickling solution was tested through a pilot plant pickling process device that simulates the commercial pickling process of nuclear fuel cladding tubes, and the pickling efficiency was analyzed through AFM analysis of the roughness of the cladding tube surface.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2015.05a
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• pp.154-154
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• 2015

현재 액체로켓 엔진 연소기 내벽은 bonding layer NiCrAlY과 Top layer $ZrO_2$가 플라즈마 용사 방식으로 형성 된다. 이는 뛰어난 열 차폐 특성과 작업시간이 짧은 장점이 있지만, bonding layer와 Top layer 사이의 열팽창 계수 차이로 인한 균열 발생 가능성이 내재 되어 있고, 연소실 내벽에 균일한 두께의 코팅층을 형성하기 어렵고 설비가 비싸다는 단점으로 인하여 세라믹 코팅 층을 금속 코팅 층으로 대체 하고자 한다. 금속 코팅층은 모재와의 밀착성이 높고, 우수한 산화 및 부식방지 기능을 가지며 저렴하다는 장점이 있다. 또한 코팅 후 연마 작업이 가능해 연소실 내부형상을 설계조건 대로 유지 할 수 있는 특징이 있다. 따라서 본 연구에서는 연소실 내벽에 적용할 모재, 무전해 Ni-P 도금과 전해 Cr 도금층 사이의 밀착력 향상을 위한 방법에 대한 연구를 하였다. 밀착력 향상을 위한 요소로 전처리 용액과 열처리 시간에 따른 영향을 알아보고자 하였으며, 이를 위해서 5가지의 산세 용액으로 각 시편을 산세 한 후, 6시간, 12시간, 18시간 열처리 하여 단면을 비교하여 열처리에 영향을 알아보고자 하였다. 연구 결과 산세 용액의 영향은 크게 나타나지 않았으며, 열처리 시간이 길수록 Ni-P/Cr의 확산이 더 잘 일어나 확산층이 더 넓어지면서 밀착력이 더 좋아 진 것으로 판단되어 진다.

• Resources Recycling
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• v.20 no.1
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• pp.61-68
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• 2011

Impurity removal from metallurgical grade silicon by acid washing at $50^{\circ}C$ was investigated by employing sulfuric, nitric acid and the mixture of hydrochloric and hydrofluoric acid. Acid washing treatment had no effect on the removal of boron and the concentration of this clement after treatment was rather increased. In our experimental range, the removal percentage of phosphorus was 60%. In the acid washing with sulfuric and nitric acid, the removal percentage of major impurities was below 50%, which indicates that refining effect was not great with these acids. Acid washing with the mixture of hydrochloric and hydrofluoric acid led to removal percentage of higher than 90%. Data on the purity of silicon after acid washing at various conditions are reported.

• Resources Recycling
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• v.17 no.2
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• pp.36-45
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• 2008

Pickling of oxidized 304 stainless steel has been investigated using rotating disk electrode in waste acid solutions generated from the etching process of silicon wafer in order to recycle them. The waste acid solution contained acetic, nitric, hydrofluoric acids, and silicon of $19.6g/L^{-1}$. Electrochemical behavior during the pickling was distinctively different between the original and silicon-removed acid solutions. Open circuit potential was continuously changed in the original solution, while it was discontinuously changed and fluctuated in the silicon-removed solution. Fast and abrupt removal of surface oxide layer with severe pitting was observed in the silicon-removed solution. It was found that solution temperature had the most influential effect on glossiness. Surface glossiness after pickling was decreased with solution temperature. At the same condition, the glossiness was higher in the original solution than in the silicon-removed solution.

• Clean Technology
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• v.2 no.1
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• pp.96-108
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• 1996

$NO_x$ is mainly emitted from mixed acid pickling process in the stainless industry and its impact to the environment has been worried over. This study which may be considered as one of the development of clean technologies, differing from the traditional end pipe technology is about how to reduce $NO_x$ emission through the modification of corresponding process. This study consists of two parts. First, the influence of various reaction parameters in a acid pickling process on $NO_x$ emission was investigated. Second, the influence of hydrogen peroxide on $NO_x$ formation, which is known as inhibitor of $NO_x$ emission, was investigated. Major findings in this study are as follows. The important reaction parameters which have a great influence on $NO_x$ emission are the reaction temperature and the concentration of fluoric acid. The concentration of nitric acid, some of which results in $NO_x$ compound is not as important as the concentration of fluoric acid. Synthetic mixed acid of nitric acid and fluoric acid itself in absent of pickling plate contributed the $NO_x$ emission, however, its impact was negligible in terms of quantity. The addition of hydrogen peroxide to the acid pickling process significantly contributed to the reduction of $NO_x$ emission and successfully achieved 80% reduction of $NO_x$ emission at the condition of $9.51{\times}10^{-2}mole\;hydrogen\;peroxide/m^2$ pickling area. This result was compared to literature value from Avesta steel process, indicating a sixth of hydrogen peroxide addition of Avesta's in achieving a same amount of $NO_x$ reduction. The region of the economic hydrogen peroxide addition per unit area of plate to be pickled from the result of this study was established.

• Resources Recycling
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• v.26 no.6
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• pp.29-37
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• 2017

Nuclear fuel cladding tube is fabricated by pilgering and annealing process. In order to remove impurity and oxygen layer on the surface, pickling process is carried out. When Zirconium(Zr) is dissolved and saturated in acid solution during the pickling process, all the waste acid including Zr is disposed. Therefore, $BaF_2$ is added into the waste acid to extract Zr and $Ba_2ZrF_8$ is subsequently formed. To recycle Zr by electrowinning process, $Ba_2ZrF_8$ is used as electrolyte, but it has high melting point ($1053^{\circ}C$). $ZrF_4$ should be added into $Ba_2ZrF_8$ to decrease the melting point. In this paper, it was investigated that $Ba_2ZrF_8$ was separated to $BaF_2$ and $ZrF_4$ by vacuum distillation. Firstly, $BaF_2$ with different particle size ($1{\mu}m$, $35{\mu}m$, $110{\mu}m$) was added into the waste acid and the respective precipitation property was estimated. $BaF_2$ obtained by vacuum distillation was shattered by ball-milling with different time. The precipitation efficiency was compared with $1{\mu}m$ of ${BaF_2}^{\prime}s$ one, which was not used as precipitation agent.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2013.05a
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• pp.71-71
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• 2013

AZ31 마그네슘 합금 판재는 경량화가 요구되는 분야에 사용되는 것을 목표로 설계되어 상업화가 추진되고 있으며, 이의 적용을 위해서는 마그네슘 판재의 내 부식성을 제어하는 표면처리 공정이 필수적이다. 표면처리에서는 강판 및 알루미늄판재의 표면처리 공정에 이용되는 화성처리-전착도장 공정에 따라야 하겠지만, 산 용액에 매우 취약한 마그네슘 소재의 특성상 같은 처리 조건을 적용하기 어렵다. 산 종류에 따른 AZ31 마그네슘합금판재 표면처리효과를 알아보기 위해 여러 종류의 산 처리 후 내 부식성을 알아보고 HH(Heat and Humidity; 가압, 가습 조건에서 열처리) 공정을 접목시킨 표면처리 결과에 대하여도 관찰하였다. 그 중 불산을 이용한 표면처리는 농도별로 진행하여 산세의 농도가 표면에 주는 영향에 대하여도 알아보았다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.127-127
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• 2016

일반적인 알루미늄 표면처리 방식중 De Smut 는 질산 50~60% 용액에 상온에서 수초에서 수분 침적으로 Smut가 거의 제거가 되므로 도금공정에서 문제가 되지않았다. 단지 NOx 의 발생으로 작업공간 에서의 환경이 열악해 질 수 있다는 것이 문제 였다, 그러나 환경문제에 있어서 정부의 질소 규제 가 시작 되면서 알루미늄을 재료로 표면처리 하는 업체 에서는 질산 사용이 곤란해 해졌다. 그러나 질산이 금속과 의 친화력은 스테인레스, 알루미늄, 등 많은 금속에서 소지금속의 용해를 방지 하면서 산화스케일( De Smut)을 제거하는 데 유용한 산이어서 아직도 이용되고 있는 실정이다. 본 연구에서 는 우선 스테인레스 강의 산세시 불산과 질산의 혼산을 사용 하는 것을 불산, 불화암모늄, 황산, 과산화 수소 혹은 불산, 염산, 과산화 수소 등으로 전환 사용 하는 것 에 착안 하여 황산, 과산화수소 시스템에서 혹은 불산, 황산, 과산화 수소, 등으로 Smut 제거가 가능 한지 알아보고 그 효과를 살펴보았다.

• Resources Recycling
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• v.5 no.2
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• pp.57-62
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• 1996

The regeneration of wastc piddlng acid from ironmaking industry produces Iron oxides as by products which are used for pigments and raw matcrial of ferrite. Thc impurilies level of iron axides for ferrile arc strictly regalated. Filtrat~on, adsorption medw technique, Fe leaching and ncutralizaiion wcre tried in order to remove silica impurities in the wasb pickling acid solution.