• Applied Science and Convergence Technology
• /
• v.27 no.1
• /
• pp.9-13
• /
• 2018

Samples of anodic oxide film used in semiconductor and display manufacturing processes were prepared at different electrolyte temperatures to investigate the corrosion resistance. The anodic oxide film was grown on aluminum alloy 6061 by using a sulfuric acid ($H_2SO_4$) electrolyte of 1.5 M at $0^{\circ}C$, $5^{\circ}C$, $10^{\circ}C$, $15^{\circ}C$, and $20^{\circ}C$. The insulating properties of the samples were evaluated by measuring the breakdown voltage, which gradually increased from 0.43 kV ($0^{\circ}C$) to 0.52 kV ($5^{\circ}C$), 1.02 kV ($10^{\circ}C$), and 1.46 kV ($15^{\circ}C$) as the electrolyte temperature was increased from $0^{\circ}C$ to $15^{\circ}C$, but then decreased to 1.24 kV ($20^{\circ}C$). To evaluate the erosion of the film by fluorine plasma, the plasma erosion and the contamination particles were measured. The plasma erosion was evaluated by measuring the breakdown voltage after exposing the film to $CF_4/O_2/Ar$ and $NF_3/O_2/Ar$ plasmas. With exposure to $CF_4/O_2/Ar$ plasma, the breakdown voltage of the film slightly decreased at $0^{\circ}C$, by 0.41 kV; however, the breakdown voltage significantly decreased at $20^{\circ}C$, by 0.83 kV. With exposure to $NF_3/O_2/Ar$ plasma, the breakdown voltage of the film slightly decreased at $0^{\circ}C$, by 0.38 kV; however, the breakdown voltage significantly decreased at $20^{\circ}C$, by 0. 77 kV. In addition, for the entire temperature range, the breakdown voltage decreased more when sample was exposed to $NF_3/O_2/Ar$ plasma than to $CF_4/O_2/Ar$ plasma. The decrease of the breakdown voltage was lower in the anodic oxide film samples that were grown slowly at lower temperatures. The rate of breakdown voltage decrease after exposure to fluorine plasma was highest at $20^{\circ}C$, indicating that the anodic oxide film was most vulnerable to erosion by fluorine plasma at that temperature. Contamination particles generated by exposure to the $CF_4/O_2/Ar$ and $NF_3/O_2/Ar$ plasmas were measured on a real-time basis. The number of contamination particles generated after the exposure to the respective plasmas was lower at $5^{\circ}C$ and higher at $0^{\circ}C$. In particular, for the entire temperature range, about five times more contamination particles were generated with exposure to $NF_3/O_2/Ar$ plasma than for exposure to $CF_4/O_2/Ar$ plasma. Observation of the surface of the anodic oxide film showed that the pore size and density of the non-treated film sample increased with the increase of the temperature. The change of the surface after exposure to fluorine plasma was greatest at $0^{\circ}C$. The generation of contamination particles by fluorine plasma exposure for the anodic oxide film prepared in the present study was different from that of previous aluminum anodic oxide films.

• Transactions of the Korean hydrogen and new energy society
• /
• v.7 no.1
• /
• pp.81-92
• /
• 1996

The Ar/Ar-$H_2$ plasma method was applied to reduce oxides and refine metals of V, Ta and B. In addition, the high temperature chemical reaction in Ar plasma and of the refining reaction in the Ar-(20%)$H_2$ plasma were analyzed. The crude V of 96wt% purity was obtained at the ratio of $C/V_{2}O_{5}=4.50$ by the Ar plasma reduction grade and the maximum reduction was obtained at $C/V_{2}O_{5}=4.50$ due to the $O_{2}$ loss from the thermal decomposition of vanadium oxide. In the Ar-(20%)$H_2$ plasma refining, the metallic V of 99.2wt% was produced at the ratio of $C/V_{2}O_{5}=4.40$. It was considered that a main refining reaction resulted from the chemical reaction between the residual carbon and residual oxygen. The metallic Ta of 99.8wt% was obtained at the ratio of $C/Ta_{2}O_{5}=5.10$ in a Ar plasma reduction and the Oz loss from the thermal decomposition of tantalum pentoxide did not take place. The deoxidation reaction was more significant than the decarburization reaction in the Ar-(20%)$H_2$ plasma refining and the metallic Ta of 99.9wt% was produced within the range of $C/Ta_{2}O_{5}$ ratio of 4.50 to 5.10. The Vickers hardness of Ta in the above mentioned range was about 220Hv due to the decrease in a residual oxygen by the deoxidation reaction. On the other hand, C is no suitable agent for the reduction of $B_{2}O_{3}$ by the Ar and Ar-$H_2$ plasma. But Fe-B-Si alloy was produced with the reduction of $B_{2}O_{3}$ in the melt when Fe, C, $B_{2}O_{3}$, and ferroboron mixtures were melted by the high frequency induction melting.

• Korean Journal of Heritage: History & Science
• /
• v.46 no.1
• /
• pp.208-227
• /
• 2013

Twenty-seven bronze bowls excavated from the Goryo burial complex at Deobu-gol were examined for their microstructure and chemical composition to characterize the bronze technology practiced by commoners at the time. Results showed that the objects examined can be classified into four groups: 1) objects forged out of Cu-near 22%Sn alloys and then quenched; 2) objects cast from Cu-below 10% Sn alloys containing lead; 3) objects cast from Cu-10%~20% Sn alloys containing lead and then quenched; 4) objects forged out of Cu-10~20% Sn alloys containing lead and then quenched. This study revealed that the fabrication technique as determined by alloy compositions plays an important role in bronze technology. The use of lead was clearly associated with the selection of quenching temperatures, the character of inclusions and the color characteristics of bronze surfaces. It was found that the objects containing lead were quenched at temperatures of $520^{\circ}{\sim}586^{\circ}C$ while those without lead were quenched at the range of $586^{\circ}{\sim}799^{\circ}C$. The presence of selenium in impurity inclusions was detected only in alloys containing lead, suggesting that the raw materials, Cu and Sn, used in making the lead-free alloys for the first group were carefully selected from those smelted using ores without lead contamination. Furthermore, the addition of lead was found to have significant effects on the color characteristics of the surface of bronze alloys when they are subjected to corrosion during interment. In leaded alloys, corrosion turns the surface light green or dark green while in unleaded alloys, corrosion turns the surface dark brown or black. It was found that in fabrication, the wall thickness of the bronze bowls varies depending on the application of quenching; most of the quenched objects have walls 1mm thick or below while those without quenching have walls 1mm thick or above. Fabrication techniques in bronze making usually reflect social environments of a community. It is likely that in the late Goryo period, experiencing lack of skilled bronze workers, the increased demand for bronze was met in two ways; by the use of chief lead instead of expensive tin and by the use of casting suitable for mass production. The above results show that the Goryo bronze workers tried to overcome such a resource-limited environment through technological innovations as apparent in the use of varying fabrication techniques for different alloys. Recently, numerous bronze objects are excavated and available for investigation. This study shows that with the use of proper analytical techniques they can serve as a valuable source of information required for the characterization of the associated technology as well as the social environment leading to the establishment of such technology.

• Conservation Science in Museum
• /
• v.30
• /
• pp.23-46
• /
• 2023

The Jija Chongtong Gun, owned by Seokdang Museum of Dong-A University, is a tubedstyle heavy weapon of the battlefield in the mid-Joseon Dynasty and is the second largest firearm after Cheonja Chongtong. The original surface color of the Jija Chongtong Gun was obscured by foreign substances and therefore it was judged that its condition requires the conservation treatment. For stable conservation treatment, gamma ray and X-ray non-destructive transmission surveys was conducted to determine the internal structure and conservation condition. And the component analysis on the material components and surface contaminants of Jija Chongtong Gun was conducted by utilizing the p-XRF component analysis, SEM-EDS component analysis, and XRD analysis. As a result of the gamma-ray and X-ray non-destructive transmission investigation, a large amount of air bubbles was observed inside Jija Chongtong Gun, and the part that appeared to be a chaplet by visual observation was not identified. As a result of gamma-ray and p-XRF component analysis, it was confirmed that Jija Chongtong Gun was bronze made of copper (Cu), tin (Sn), and lead (Pb) alloy. As a result of surface analysis of foreign substances using SEM-EDS, it was confirmed that the main components of white foreign substances were calcium (Ca), sulfur (S), and titanium (Ti). Titanium was presumed to be titanium dioxide (TiO₂), the main component of white correction fluid. The red foreign substance was confirmed to contain barium (Ba) as its main ingredient, and was presumed to be barium sulfate (BaSO₄), an extender pigment in paint. White and red contaminants, mainly composed of titanium and barium, are presumed to have been deposited on the surface in recent years. The yellow foreign substances were confirmed to be aluminum (Al) and silicon (Si), and were presumed to have originated from soil components. As a result of SEM-EDS and XRD component analysis, the white foreign substance was confirmed to be gypsum (CaS). Based on the results of component analysis, surface impurities were removed, stabilization treatment, and strengthening treatment were performed. During the conservation process, unknown inscriptions Woo (右), Byeong (兵), Sang (上), and Yi (二) were discovered through a portable microscope and precise 3D scanning. In addition, the carving method, depth, and width of the inscription were measured. Woo Byeong Sang is located above Happo Fortress in Changwon, and Yi can be identified as the second hill.