• KOMUNHWA
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• no.56
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• pp.147-180
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• 2000

This study has been investigated to use base research data of archaeology and conservation science for cultural properties about iron artifacts from Kimhae Yangdong-Ri tombs as metallurgical research. 1. Iron artifacts from Kimhae Yangdong-Ri tombs had be

• Journal of Conservation Science
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• v.29 no.4
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• pp.297-309
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• 2013

Iron objects become corroded at fast speed from the moment when they are excavated, so it is needed to control corrosion through processes of conservation treatment. However, re-corrosion mostly takes place in excavate iron objects, although they have already gone through the process of conservation treatment, and it is more difficult to carry out the second conservation treatment of re-corroded excavated iron objects than the first conservation treatment, and it requires a longer period of time to treat them as well. In this study, aims to discover factors of re-corrosion by scientifically analyzing corrosion products generated during the process of storage after the process of conservation treatment. The finished on conservation treatment of the iron artifacts, which were unearthed from three ancient site in Gyeongju by using the same conservation method between 2002 and 2009, re-corrosion condition observed on the packaging-iron artifacts. Focused on 9 target forged iron artifacts among them, this study analyzed the physical changes by mass measurement, naked-eye and microscopic observations and the chemical changes by SEM-EDS, XRD, IC and ICP analysis. The results show that the yellowish brown corrosion products formed on the facing surface of part dropped from the artifacts had different associated forms but acicular shape. In addition, the acicular shape became clearer as the color changed from red to yellowish brown. According to the process when the conservation treatment was completed, the mass of the artifacts increased in proportion to the corrosion products and the chloride ion ($Cl^-$) concentration had a tendency to increase relatively. ${\beta}$-FeOOH (akaganeite) was confirmed in the XRD analysis for the corrosion products of all the collected samples. As a result of ICP analysis, $Na^+$ and $Ca^{2+}$ components were confirmed.

• Journal of Conservation Science
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• v.29 no.2
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• pp.187-196
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• 2013

This study is on the corrosion of iron objects caused by sulfides in undersea environment. The corrosion state of objects in seawater and their damage state after underwater and left in highly humid air were studied. The samples of this study were four iron objects which had been taken out from undersea mud layer located in Taean Mado, Chungcheongnamdo. SEM-EDS and XRD analyse on the objects to check whether they have sulfides or not. The result of analysis suggested that the major component of corrosion product generated in undersea deposit soil is sulfur(S) and iron sulfide(FeS) is formed as sulfide. However, there was no clear corrosion on the surface of objects which was exposed to sea water because of the impact of concretion which covered the surface. In order to check the damage status of iron objects after they had been taken out of sea water, exposure tests in high humidity environment and dehumidified environment were done on the corrosion products. The result of the test suggested that the oxidization of iron sulfide corrosion product makes iron sulfate ($FeSO_4$) and sulfuric acid ($H_2SO_4$) and they can cause secondary corrosion of iron objects. Therefore, it is believed that the iron sulfide corrosion product of iron objects taken out from underwater environment should be removed by all means and the keeping environment of the iron objects should also maintain dehumidified state.

• 한국문화재보존과학회:학술대회논문집
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• 2002.02a
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• pp.45-52
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• 2002

본 연구에서는 KaOH, $K_2CO_3$, Sodium, 그리고 1차 이온수 용액의 $Cl^-$ 이온 추출량과 부식생성물의 생성순위, 부식물 생성, 그리고 부식물 제거에 관하여 관찰하였으며 이 연구로 아래와 같은 결과를 얻었다. $Cl^-$ 이온 추출량에 대한 실험 결과 NaOH은 탈염 초기에는 Cl- 이온을 잘 추출시켰으나 탈염 횟수가 증가하면서 $Cl^-$ 이온의 추출량이 급감하였다. 또한 유물 중량 변화에도 감소폭이 가장 심하였다. $K_2CO_3$은 NaOH나 1차이온수 용액과 비교해 보면 이 방법은 탈염처리동안 $Cl^-$ 이온을 꾸준히 추출시켜 주었으며 다른 탈염용액에 비해 유물 중량변화가 거의 관찰되지 않았다. Sodium 용액은 $K_2CO_3$ 용액과 마찬가지로 탈염처리 동안 $Cl^-$ 이온을 꾸준히 추출시켰으며 다른 탈염 용액에 비해 $Cl^-$ 이온 추출량이 가장 많았다. 하지만 이 용액은 약품 내에 불순물인 $Cl^-$ 이온을 $3\~5\;ppm$을 기지고 있어 보존처리자가 탈염처리를 할 때 좀 더 신중하게 생각해야 할 것 같다. 1차 이온수 용액은 부식인자가 $Cl^-$이온을 완전하게 제거해주지는 못하였지만, pH가 $7.5\~7.9$로 다른 탈염 용액에 비해서 전위차가 낮으며, 별도로 탈알칼리 처리를 하지 않아도 되기 때문에 유물손상은 극소화할 수가 있다. 따라서 이 용액은 부식이 매우 심한 철제 유물이나 균열이 많은 주조 철편과 같은 유물을 처리할 때 적절한 용액이다. 부식생성물 관찰에서는 출토 철기 유물에 생성된 부식물은 주로 인철광$(\gamma-FeOOH)$, 침철광$(\alpha-FeOOH)$, 적금광$(\beta-FeOOH)$, 그리고 자철광$(Fe_3O_4)$이다. 인위적 부식에서는 전부 인철광의 부식물이 생성되었고 자연적 부식에서는 모두 침철광의 부식물이 생성되었다. 특히 철제 표면에 자연적으로 생성된 공식 녹을 XRD 분석한 결과 적금광으로 동정되었다. 이런 모든 시편들을 각 탈염방법에 따라 탈염처리한 후 XRD와 SEM-EDS으로 분석한 결과 인철광과 침철광은 어떠한 변화도 보이지 않았고, 다만 적금광으로 동정된 시편만이 잔존하지 않았다. 철기 제작별 $Cl^-$ 이온 추출량과 탈염효과에 대한 비교 실험은 이온 크로마토그래피 분석 결과와 마찬가지로 단조 철제유물이 주조 철제보다 $Cl^-$ 이온을 많이 가지고 있었으며, 탈염 처리 후에는 $Cl^-$ 이온은 전혀 발견되지 않았다. 이상의 결과 $K_2CO_3$와 Sodium 용액은 탈염처리에서 가장 적합한 탈염처리 용액으로 알수가 있었으며 특히 어떠한 탈염 용액으로 유물을 처리한다 해도 철제유물에 생성된 부식물은 제거되지 않는다는 것을 알게 되었다. 따라서 보존처리자는 유물 표면의 부식 상태만을 보고 처리하기 보다는 철기제작물로 고려하여 처리하는 것이 필요하다. 또한 금속에 부식을 야기시키는 $Cl^-$ 이온과 부식물을 완전하게 제거하여 탈염처리를 하는 것이 유물 부식을 최대한 지연시킬 수 있는 것이라 생각된다.

• Journal of Conservation Science
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• v.30 no.1
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• pp.1-11
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• 2014

Stabilization of iron artifacts is focused on desalination than corrosion inhibitors. However artifacts are not condition of desalination treatment must be applied to corrosion inhibitors. But iron artifacts is not representative of inhibitors which drug is most effective qualities have not been identified. Therefore in this study validates the effectiveness of existing inhibitors and its purpose is to suggest corrosion inhibitors for iron artifacts. In this study, Comparative experiment of corrosion inhibitors is selected BTA, DAN and MEA, TEA. This study was studied using Corrosion resistance test, Contact angle, XPS. As a result, all the samples treated with corrosion inhibitors was formed hydrophobic coating and was rising corrosion resistance. Also, the concentration of corrosion inhibitors was 3% better than 0.3%. BTA in the XPS experiment, the corrosive material to block the CH bond of the peak concentration was highly. This is considered corrosion potential is very high to see out the effect in the polarization experiment. Ethanolamine was superior to the MEA rather than in the TEA. MEA is likely to be appropriate in an outdoor iron artifacts seem to be suitable as corrosion inhibitors.

• Journal of Conservation Science
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• v.28 no.4
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• pp.343-351
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• 2012

Excavated archaeological iron objects are prevented from being corroded going through desalination which slow down being corroded. However archaeological iron objects are liable to be corroded due to the high ionization tendency even though they are stored in environment restricted from corrosion factors. Iron objects could be deteriorated more than just excavated. Therefore this study investigated about the characteristic of re-corrosion and the effect on objects. In study, archaeological iron nails in storage for 4 years after conservation treatments were tested. Optical microscopy and X-ray photography for appearance, XRD, SEM-EDS, Raman spectroscopy for chemical composition, IC for chloride ions concentration inside iron nails were used. As results, iron nails carried out conservation treatments measured a high concentration of chloride ions after the long storage period. The form of objects were not in good condition such as broken or destroyed when the high chloride ions concentration was detected. In addition, the yellow and red powdery corrosion product were detected on the boundary between corrosion products and substrates and they were identified as akaganeite which is symptom of active corrosion.

• 보존과학연구
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• s.7
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• pp.1-10
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• 1986

• Korean Journal of Heritage: History & Science
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• v.46 no.3
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• pp.134-149
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• 2013

The Sudang-ri Site in Geumsan is considered the historic site where Baekje dominated the inland traffic route to Gaya through Geumsan and Jinan in the 5th Century. This study identified the production techniques of iron by conducting an analysis of metallographical microstructure of the artifacts such as an iron sword and an iron sickle that were excavated in Sudang-ri Site, Geumsan, one of the regions ruled by Baekje, and tried to figure out the characteristics and the technical systems of Baekje's ironmaking around the 5th Century by comparing them with other iron artifacts produced around the same time. The analysis showed that various production techniques were applied to the artifacts excavated in Sudang-ri Site, Geumsan. Depending on the production techniques, they can be divided largely into three methods: the simple shape-forging method, the steel manufacture method after forging, and the steel manufacture & heat-treatment method after forging. The iron sickle from the stone chamber tomb No. 1, which was produced only through forging, is mostly composed of soft ferrite at both edges of the blade and at the rear making the use of the weapon impractical. From this fact, it is presumed that they were produced as burial objects or ceremonial accessories for the person buried. The iron axe from the outer stone coffin tomb No. 1 and the iron swords and sickle from the outer stone coffin tomb No. 12, which were produced through the steel manufacture method after forging such as carburizing, did not go through the heat treatment such as quenching, but applied different production processes to each part. Therefore, it is deemed that they were produced as daily tools for cultivation rather than burial objects or ceremonial accessories. The production techniques following the forging process - carburizing and heat treatment - can be found on the iron swords from the outer stone coffin tomb No. 5 and the outer stone coffin tomb No. 12. The sturdy structure of the blade part and the durable structure of the rear processed with heat are deemed to have been produced as weaponry and used by the person buried. Based on the analysis of the iron artifacts excavated from Sudang-ri Site in Geumsan, the characteristics of iron production techniques were investigated by comparing them with the artifacts from Yongwon-ri Site in Cheonan, Bongseon-ri Site in Seocheon, and Bujang-ri Site in Seosan that were made around the same time as the cluster of Baekje tombs examined by the metallographical microstructure analysis of this study. For the iron artifacts analyzed here, the changes in the techniques were investigated using the iron swords common in all of the tombs. In the case of the iron swords, it was identified the heat treatment technique called tempering was applied from the 4th Century.

• Journal of Conservation Science
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• v.27 no.3
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• pp.333-344
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• 2011

Cleaning of foreign matter and corrosion products on surface among conservation treatment of iron artifacts is an important part for looking up a original form. The sand blaster is the most popular equipment when it removes the foreign matter and corrosion products on iron artifacts surface. Current foreign matter and corrosion products equipment, which mostly uses, is sand blaster. Glass dust which sprayed from sand blaster is harmful and causing environmental pollution. In order to solve these problems, we investigated the $CO_2$ snow cleaning that use a eco-friendly equipment to apply for cleaning foreign matter and corrosion products on surface of iron artifacts. It examined by using sand blaster and $CO_2$ snow cleaning to aged steel coupon and iron artifacts. In case of aged steel coupon, the result showed that the sand blaster and $CO_2$ snow cleaning methods were similar to the degrees of cleaning foreign matter and corrosion products, through surface roughness, color measurement and SEM. $CO_2$ snow cleaning applied to aged steel coupons weren't worn out the surface in comparison with sand blaster by SEM. When applied to the iron artifacts, power nozzle of the $CO_2$ snow cleaning was an excellent cleaning effect that surface wern't worn out in comparison with sand blaster. And, it showed that internal structure change of metal was no found before and after cleaning by X-ray radiography. Consequently, we confirmed that cleaning of the sand blaster and power nozzle of $CO_2$ snow cleaning were similar to the effect. But, it's very careful to use this method because of high outlet pressure of power nozzle for applying to the iron artifacts. As a result of experiments, it could be found that the cleaning methods should be selected depending on internal state of the artifacts.

• Journal of Conservation Science
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• v.26 no.4
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• pp.407-416
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• 2010

Bacteria with ability for iron reduction in the soil can use corrosion products of iron remains as energy source. The activities of this bacteria cause the change of corrosion products. As a result, it can be difficult to identify corrosion products promoting corrosion of iron remains. The purpose of this study, is to investigate the change in corrosion products that bacteria causes and to improve understanding about the corrosion of iron remains. To simulate corroded condition of excavated iron remains, carbon steel corroded by solution of NaCl and $Na_2SO_4$ was prepared. Then the prepared carbon steel was immersed in a liquid medium with bacteria. The incubation period was 42days. After experiment, the carbon steel was analyzed by SEM-EDS, X-ray diffraction method. The result is that the carbon was changed to green because of activity of bacteria and that the plate crystal and lozenge crystal were generated on the corrosion specimen. Also, we confirmed that the activities of bacteria differenciated colors and forms of corrosion products.