• Journal of the Mineralogical Society of Korea
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• v.19 no.4 s.50
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• pp.383-392
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• 2006

Calcium carbonate stone deterioration has been intensified in urban area, mainly due to the action of atmospheric pollutant. Samples from the black surface layer were examined under petrographic and scanning electron microscope, coupled with energy dispersive X-ray analyser X-ray fluorescence and X-ray diffraction analysis was also carried out for chemical composition and mineral phase analysis, respectively. Moreover, sulphur isotope ratio was measured, in order to identify the origin of sulphate compounds in the black surface layer. Optical and electronic petrographic analysis indicated that gypsum and Quartz were contained in the black surface layer and led to microcracks. Microstructure and chemical composition analysis showed that the interface between black layer and original stone is not black but its characteristic is similar to black layer The results indicated that during deterioration process the black layer can be expanded gradually into the interface by adsorption of atmospheric pollutants. The sulphur isotope analysis demonstrates that there are different origins of the sulphur component in black surface layer.

• Journal of Conservation Science
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• v.20
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• pp.55-65
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• 2007

Black surface layers collected from stone pagodas were analyzed to study the effects of carbon compounds on the blackening of stone surface layer. The total amounts of carbon was measured through elemental analyser. Organic and elemental carbon were measured by combustion ihrornatographic $CO_2$ determination after elimination of carbonates carbon with acid treatment. The elemental carbon concentration in the black surface layer measured 0.52wt.%. This value is not sufficient to explain the complete blackening of stone surface. To trace the origin of carbon in black surface layer on the stone pagoda, aerosol samples for PM 10 were collected at the near sites of the pagoda. The major components of them were soluble ions(42.8wt.%), carbon(38.4 wt.%) and crustal matter(16wt.%). From the high content(13wt.%) of elemental carbon in aerosol ran be deduced that it may be a prime origin for the elemental carbon in the black surface layer on the stone pagoda. The crustal matter in aerosol can be also a origin of silicate mineral in black surface layer and plays a important role in the darkening of black surface layer.

• Journal of the Mineralogical Society of Korea
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• v.17 no.1
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• pp.75-83
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• 2004

Blackening on stone monuments is serious problem, because it is not only aesthetically unattractive, but also an important process in stone deterioration. Black surface layers contain often a large amounts of iron compound. Therefore it is assumed that besides another elements the iron have influence on blackening of surface. After the samples of black surface layers were collected from the stone monuments (Museumsinsel) in Berlin, Germany, especially in this study has been used Mossbauer spectroscopy in order to determine the valence and chemical composition of iron. Mineralogical and chemical analyses were carried out X-ray diffractormetry and X-ray fluorescence method on the black surface layer's samples and original stone samples. The origin of Iron compound in the black surface provides the important clue for the conservation work of stone monuments, like removing of black surface. To find it, black surface layer on white sandstone -it contains very small amount of iron compound- was compared with that on the red sandstone (Fe contains very small amount of iron compound- was compared with that on the red sandstone (Fe abundant). As a results, it is assumed that the iron in black layer on white sandstone is originated mainly from a surrounding environmental material and for the iron in black layer on the red sandstone is responsible the original stone. Even if black surface layer was removed from the red sandstone, some other conservation method should be studied beyond removing of black surface layer, because the iron can move continuously from the inner zone of original stone to surface area.

• Journal of the Korean Society for Heat Treatment
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• v.8 no.1
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• pp.44-52
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• 1995

The specimen for laser hardening have been carried out using SM45C which is coated with black paint or graphite for better absorption. Segmented mirror was used in order to produce a square beam ($10{\times}10mm$) at the surface with a homegeneous intensity distribution across the beam. $CO_2$-Laser power was changed from 2kW to 4kW and transfer velocity was varied from 0.1m/min to 2.0m/min. The maximum hardness and case depth of SM45C steel are 790Hv and 1.5mm by laser hardening. When the surface of specimens was melted during laser hardening. the surface hardness of SM45C steel was decreased. The surface hardness of 2 layer coated specimen(black paint: $15.4{\mu}m$, graphite coating: $9.5{\mu}m$) was increased than that of 1 layer coated specimen. It is desirable to prepare 2 or more coating layer on the steel surface in order to sufficient case depth and hardness in laser hardening. The graphite coating on the specimen surface was obtained more uniform temperature distribution than black paint coating in laser hardening process.

• Journal of the Korean institute of surface engineering
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• v.32 no.3
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• pp.312-316
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• 1999

The interfacial structure of duplex treated AISI 4140 consisting of iron nitride and TiN layer was characterized by optical microscope, SEM and XRD. A black layer was formed from the decomposition of iron nitride during Ti ion bombardment. The black layer was characterized as an a-Fe phase transformed from the iron nitride by XRD. In order to identify the formation mechanism of the black layer, a thermal analysis of iron nitride undertaken by DSC method. As an iron nitride was mostly consisted of ${\gamma}$'-Fe$_4$N and $\varepsilon$-$Fe_3$N phase after plasma nitriding, in this study, a ${\gamma}$'$-Fe_4$N and $\varepsilon$-$Fe_3$N powders were separately prepared by the different processing conditions of gas nitriding of iron powder in the fluidized bed. From the DSC thermal analysis, the phase transformation of ${\gamma}$'$-Fe_4$N, $\varepsilon$-$Fe_3$N was followed the path of transformation; $ \Upsilon{'}-Fe_4$Nlongrightarrow${\gamma}$-Felongrightarrowa-Fe and of $\varepsilon$-$Fe_3$Nlongrightarrow$\varepsilon$-$Fe_{2.5}$ /N+${\gamma}$'$-Fe_4$Nlongrightarrow${\gamma}$'-Fe$_4$Nlongrightarrow${\gamma}$longrightarrowFelongrightarrowalongrightarrowFe, respectively. It explains the reason why the $\varepsilon$ $-Fe_3$N phase disappeared in the first time and then ${\gamma}$'-Fe$_4$N in the formation of the black layer in the duplex coating.

• Journal of the Korean institute of surface engineering
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• v.32 no.6
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• pp.647-657
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• 1999

Due to the inherently poor adhesion strength of Cu-based leadframe/EMC (Epoxy Molding Compound) interface, popcorn cracking of thin plastic packages frequently occurs during the solder reflow process. In the present work, in order to enhance the adhesion strength of Cu-based leadframe/EMC interface, black-oxide layer was formed on the leadframe surface by chemical oxidation of leadframe, and then oxidized leadframe sheets were molded with EMC and machined to form SDCB (Sandwiched Double-Cantilever Beam) and SBN (Sandwiched Brazil-Nut) specimens. SDCB and SBN specimens were designed to measure the adhesion strength between leadframe and EMC in terms of critical energy-release rate under quasi-Mode I ($G_{IC}$ ) and mixed Mode loading ($G_{C}$ /) conditions, respectively. Results showed that black-oxide treatment of Cu-based leadframe initially introduced pebble-like X$C_2$O crystals with smooth facets on its surface, and after the full growth of $Cu_2$O layer, acicular CuO crystals were formed atop of the $Cu_2$O layer. According to the result of SDCB test, $Cu_2$O crystals on the leadframe surface did not increase ($G_{IC}$), however, acicular CuO crystals on the $Cu_2$O layer enhanced $G_{IC}$ considerably. The main reason for the adhesion improvement seems to be associated with the adhesion of CuO to EMC by mechanical interlocking mechanism. On the other hand, as the Mode II component increased, $G_{C}$ was increased, and when the phase angle was -34$^{\circ}$, crack Kinking into EMC was occured.d.

• Journal of the Microelectronics and Packaging Society
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• v.15 no.3
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• pp.27-33
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• 2008

With increasing use of portable appliances such as PDA and cellular phone, changing environment of applications requires higher solder joint reliability. The ENIG (Electroless Nickel Immersion Gold) process has been widely used for fine pitch SMT (Surface Mount Technology) and BGA (Ball Grid Array) packaged devices due to its benefits including excellent solderability, high uniformity and substantial legibility throughout the packaging process. Its brittle fracture of solder, however, has received increasingly attentions. It was Down that fracture brittleness is mainly related with black pad resulting from galvanic nickel corrosion and P-enriched layer formation between the IMC (Intermetallic Compounds) and electroless nickel layer. Theoretically, smooth electroless Ni layer was blown to have a advantages in minimizing the black pad phenomenon by uniform solution exchange during immersion gold plating. Nevertheless, how to control the surface morphology of electroless Ni layer has been hardly blown. This study investigates an effect of surface morphology of Cu underlayer on surface morphology of electroless Ni layer. To obtain various kinds of surface morphology of Cu layer, two types of Cu etching chemical and a number of Cu etching treatment were applied.

• Journal of the Korean Society for Heat Treatment
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• v.15 no.5
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• pp.213-218
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• 2002

In order to develop the economic and environmental water-soluble black coloring agent, some adequate chemical mixtures were mixed and this solution was applied to coat quenched and tempered 51B20 steel bolt. Some basic properties of the solution and characteristics of the coated film in addition to the corrosion resistance were investigated. The developed 100 kg of water-soluble black coloring agent solution was a chemical mixture consisted of 10 kg of aqueous coloring agent, 40 kg of surface active agent, 0.3 kg of anti-foam agent and $50{\ell}$ of water. The coated film of the bolt was composed of hard layer of about $2{\mu}m$ and the disbondable soft layer of about $4{\mu}m$ above the hard layer. Many surface active agents peaks and a few hydrophilic peaks were observed in the coated film. Surface roughness value of the coated bolt was lower than that of the non-coated bolt. Corrosion resistance of the coated bolt considerably improved and also relatively showed a good polarization resistance at test condition of $40^{\circ}C$ colorizing temperature and 5% the solution concentration in 3% NaCl anodic polarization test. Initial appearance time of the surface rust was greatly retarded owing to the coated film in salt spray test.

• Journal of the Korean institute of surface engineering
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• v.40 no.1
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• pp.32-38
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• 2007

Ni coating layers were formed using a newly developed electroless Ni plating solution. The properties of Ni coating layer such as internal stress, hardness, surface roughness, crystallinity, solderability and surface morphology were investigated using various tools. Results revealed that internal stress decreased with plating time and reached $40N/mm^2$ at 20 minutes of the plating time. Hardness increased with increasing P content and thickness. Surface roughness of the pad decreased with Ni and Ni/Au plating. Crystallinity decreased with increasing P content. Solderability based on wettability decreased with Ni and Ni/Au plating. Based on surface morphology, it is expected that Ni coating layer formed using a newly developed electroless Ni plating solution is lower than that formed using a commercial electroless Ni plating solution in possibility of black pad occurrence.

• Journal of Conservation Science
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• v.37 no.2
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• pp.77-89
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• 2021

In this study, materials and color formation techniques were assessed for black potteries excavated from the Janghyeon-dong, Jungsan-dong and Gyodong-ri sites during the Proto-Three Kingdoms period in Ulsan, Korea. Although the black potteries were black superficially, the inner cores were either black or reddish yellow. Microscopy analysis identified that body clay was used for reddish iron oxide rich soils with quartz, alkali feldspar and mica, along with grains of myrmechite texture. Additionally, as marginal differences exist in the contents of SiO₂, Fe₂O₃ and CaO, the composition of the host rock and clay distributed around the sites was affected. Thus, we can deduce that pottery was made by soiling at a short distance. Raman spectroscopy results revealed that the black layer of the black pottery was used as amorphous combustion carbon. In addition, as a transparent layer of brown lacquer was observed on the substrate that was in contact with the surface layer, the black layer of the pottery induced black color development by a combination of combustion carbon and lacquer. Based on the mineral composition and microtexture of the body clay, the firing temperature of the potteries seemed to range from 750 to 850℃, whereas the lacquer layer was pyrolyzed at 468℃ by thermal analysis. Therefore, a combined layer of combustion carbon and lacquer, which formed the black color, was painted after the body clay was fired.