The application of infrared heating in the hot press forming of the thermoplastic composites is conducive to productivity with high-speed heating. However, high energy, high forming temperature, and high-speed heating derived from infrared heating can cause material degradation and deteriorate properties such as re-melting performance. Therefore, this study was conducted to optimize the process conditions of the hot press forming suitable for carbon fiber reinforced polyetherketoneketone(CF/PEKK) composites that are actively researched and developed as high-performance aviation materials. Specifically, the degradation mechanisms and properties that may occur in infrared high-speed heating were evaluated through morphological and thermal characteristics analysis and mechanical performance tests. The degradation mechanism was analyzed through morphological investigation of the crystal structure of PEKK. As a result, the size of the spherulite decreased as the degradation progressed, and finally, the spherulite disappeared. In thermal characteristics, the melting temperature, crystallization temperature and heat of crystallization tend to decrease as degradation progresses, and the crystal structure disappeared under long-term exposure at 460℃. In addition, the low bonding strength was observed on the degraded surface, and the bonding surfaces of PEKK did not melt intermittently. In conclusion, it was confirmed that the CF/PEKK composite material degraded at 420℃ in the infrared high-speed heating. Furthermore, the spherulite experienced morphological changes and the re-melting properties of thermoplastic materials were degraded.
Jin, Xinghan;Haider, Muhammad Zeeshan;Park, Min-Woo;Hu, Jong-Wan
KSCE Journal of Civil and Environmental Engineering Research
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v.43
no.5
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pp.555-566
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2023
In this study, a composite phase change material (CPCM) produced using the SOL-GEL technique was developed as a thermal energy storage medium for low-temperature applications. Tetradecane and activated carbon (AC) were used as the core and supporting materials, respectively. The tetradecane phase change material (PCM) was impregnated into the porous structure of AC using the vacuum impregnation method, and a thin layer of silica gel was coated on the prepared composite using the SOL-GEL process, where tetraethyl orthosilicate (TEOS) was used as the silica source. The thermal performance of the CPCM was analysed using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). DSC results showed that the pure tetradecane PCM had melting and freezing temperatures of 6.4℃ and 1.3℃ and corresponding enthalpies 226 J/g and 223.8 J/g, respectively. The CPCM exhibited enthalpy of 32.98 J/g and 27.7 J/g during the melting and freezing processes at 7.1℃ and 2.4℃, respectively. TGA test results revealed that the AC is thermally stable up to 500℃, which is much higher than the decomposition temperature of the pure tetradecane, which is around 120℃. Moreover, in the case of AC-PCM and CPCM thermal degradation started at 80℃ and 100℃, respectively. The chemical stability of the CPCM was studied using Fourier-transform infrared (FT-IR) spectroscopy, and the results confirmed that the developed composite is chemically stable. Finally, the surface morphology of the AC and CPCM was analysed using scanning electron microscopy (SEM), which confirmed the presence of a thin layer of silica gel on the AC surface after the SOL-GEL process.
Park Seungwon;Shin Yongbi;Park Jinho;Lee Sujin;Park Woonji;Lee Huisung
Conservation Science in Museum
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v.29
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pp.1-32
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2023
The Paintings of a 60th Wedding Anniversary Ceremony Created by an Unknown Painter (Deoksu 6375), housed by the National Museum of Korea, is a five-panel painting book depicting scenes from a wedding ceremony. Hoehonrye is a type of repeated wedding ceremony to commemorate a couple's 60th wedding anniversary with congratulations from the community. The paintings of the book record five scenes from the wedding: jeoninrye, a ceremony where the groom brings a wooden wild goose to the bride's house; gyoberye, the groom and the bride bowing to each other; heosurye, pouring liquor to toast to the couple's longevity; jeopbin, offering tea to guests; and a banquet to celebrates the couple's 60th wedding anniversary. The book describes figures, buildings and a variety of items in detail with delicate brushstrokes. The techniques were examined using microscopy, infrared, and X-ray irradiation and hyperspectral imaging analysis. The invisible parts were examined to identify the rough sketch and distinguish pigments and dyes used for each color. The components of the pigments were determined by X-ray fluorescence analysis, while the dyes were identified by UV-vis spectrometry. Microscope observation revealed that the fabric used for the paintings was raw silk thread with almost no fiber twist, and plain silk fabric. Hyperspectral imaging analysis, X-ray fluorescence analysis, and UV-vis spectrometry confirmed that the white pigment was white lead and the black was chinese ink. The red pigments were using red clay, cinnabar, and a mixture of cinnabar and minium. Brown was made using red clay and organic dyes, and yellow using gamboge. Green was identified as indigo, malachite, chrome green, barium sulfide, and blue as azurite, smalt, and indigo. The purple dye was estimated as a mixture of indigo and cochineal, and gold parts were used gold powder. Hyperspectral images were distinguished parts damaged and conservation treatment area.
The test answer sheets submitted by examinees in the Joseon Dynasty were called Sigwon (test papers with answers, 試卷), and Siji (blank test papers, 試紙) were generally prepared by the examinees themselves. At that time, paper was not produced as a standard product, so there was no uniformity in size or manufacturing method. Mulberry paper in the Joseon Dynasty was basically transparent, so various paper processing methods were applied for examinees to write answers on both sides. In order for ink lines to be written smoothly, Dochim (hitting paper with a wooden bat on the stone, 搗砧) or surface processing was treated. We found a 19th-century Siji (試紙) that was processed in a unique way, which led to this study. An unusual Sigwon (試卷) is one by Lee Mangi (李晩耆) from 1848 owned by the National Folk Museum of Korea. We found that an opaque white substance was thickly applied between the papers of this Siji (試紙). Through component analysis using infrared spectrophotometry, fluorescence X-ray spectroscopy, optical and polarizing microscopy, and electron microscopy, this white substance was proved to be rice starch. From these analyses, it is presumed that this Siji (試紙) was made by soaking rice flour in water to remove a significant amount of protein, and then applying wet starch containing a small amount of protein between sheets of paper. In addition, with a Siji (試紙) reproduction experiment, we found that the paper reproduced by this processing method was thick and high in whiteness and opacity. This is believed to be a production method designed to produce double-sided paper without using multiple sheets of paper, which was difficult to obtain at that time. In this study, the material processed between the sheets of paper was disclosed only from < Lee Mangi (李晩耆)'s Sigwon (試卷)(Minsok 71745)>, but this appears to be one of several processing methods to treat the paper during the Joseon Dynasty. We hope that more similar Sigwons will be discovered in the future and that extensive research on processing methods will be conducted.
Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
/
v.15
no.1
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pp.15-26
/
2017
Cobalt ferrocyanide (CoFC) or nickel ferrocyanide (NiFC) magnetic nanoparticles (MNPs) were fabricated for efficient removal of radioactive cesium, followed by rapid magnetic separation of the absorbent from contaminated water. The $Fe_3O_4$ nanoparticles, synthesized using a co-precipitation method, were coated with succinic acid (SA) to immobilize the Co or Ni ions through metal coordination to carboxyl groups in the SA. CoFC or NiFC was subsequently formed on the surfaces of the MNPs as Co or Ni ions coordinated with the hexacyanoferrate ions. The CoFC-MNPs and NiFC-MNPs possess good saturation magnetization values ($43.2emu{\cdot}g^{-1}$ for the CoFC-MNPs, and $47.7emu{\cdot}g^{-1}$ for the NiFC-MNPs). The fabricated CoFC-MNPs and NiFC-MNPs were characterized by XRD, FT-IR, TEM, and DLS. The adsorption capability of the CoFC-MNPs and NiFC-MNPs in removing cesium ions from water was also investigated. Batch experiments revealed that the maximum adsorption capacity values were $15.63mg{\cdot}g^{-1}$ (CoFC-MNPs) and $12.11mg{\cdot}g^{-1}$ (NiFC-MNPs). Langmuir/Freundlich adsorption isotherm equations were used to fit the experimental data and evaluate the adsorption process. The CoFC-MNPs and NiFC-MNPs exhibited a removal efficiency exceeding 99.09% for radioactive cesium from $^{137}Cs$ solution ($18-21Bq{\cdot}g^{-1}$). The adsorbent selectively adsorbed $^{137}Cs$, even in the presence of competing cations.
A study was carried out to investigate the composition of rock-forming minerals and mineralogical characteristics of the five major parent rocks in Korea. The identification was done through the analyses of chemical. X-ray diffraction, thermal(DTA, TG), infrared spectroscopic, and microscopic methods. Among these methods, X-ray diffraction was considered to be the most rapid and effective way to identify minerals in the parent rocks. The main rock-forming minerals of the parent rocks were feldspars, quartz, and micas in granite and granite-gneiss, calcite and dolomite in limestone, quartz and calcite in shale, plagioclase and augite in basalt. A small amount of sesquioxides was identified as a accessory mineral by means of DTA from the parent rocks of Weoljeong series(granite) and Cheongsan series(granite-gneiss). The abrasion pH affecting the soil formation ranged from 7.5 to 8.4 in the parent rocks containing ferromagnesian minerals and carbonates. In the granite and granite-gneiss of which the main rock-forming minerals were feldspars and quartz with low content of biotite, the abrasion pH ranged from 6.2 to 6.4. In chemical composition of the parent rocks, Si, AI, and K oxides tented to increase with higher contents of quartz, feldspars, and muscovite, while Fe and Mg oxides with higher content of biotite, chlorite, amphiboles, and augite. Higher ignition loss in limestone and shale resulted in the release of $CO_2$ from calcite and/or dolomite.
A new mineral, Zn analogue of rancieite (Chimooite), has been discovered at the Dongnam mine, Korea. It occurs as compact subparallel finegrained flaky or acicular aggregates in the massive manganese oxide ores which were formed by supergene oxidation of rhodochrositesulfide ores in the hydrothermal veins trending NSN25E and cutting the Pungchon limestone of the Cambrian age. The flakes of chimooite are 0.2 mm for the largest one, but usually less than 0.05 mm. The acicular crystals are elongated parallel to and flattened on (001). This mineral shows gradation to rancieite constituting its marginal part, thus both minerals are found in one and the same flake. Color is bluish black, with dull luster and brown streak in globular or massive aggregates. Cleavage is perfect in one direction. The hardness ranges from 2.5 to 4. Under reflected light it is anisotropic and bireflectant. It shows reddish brown internal reflection. Chemical analyses of different parts of both minerals suggest that rancieite and chimooite constitute a continuous solid solution series by cationic substitution. The empirical chemical formula for chimooite has been calculated following the general formula, $R_2_{x}$ M $n^{4+}$$_{9x}$$O_{18}$$.$n$H_2O$ for the 7 $\AA$ phyllomanganate minerals, where x varies from 0.81 to 1.28 in so far studied samples, thus averaging to 1.0. Therefore, the formula of Znrancieite is close to the wellknown strochiometric formula $_Mn_4^{4+}$$O_{9}$$.$4$H_2O$. The mineral has the formula (Z $n_{0.78}$N $a_{0.15}$C $a_{0.08}$M $g_{0.01}$$K_{0.01}$)(M $n^{4+}$$_{3.98}$F $e^{3+}$$_{0.02}$)$_{4.00}$$O_{9}$$.$3.85$H_2O$, thus the ideal formula is (Zn,Ca)M $n^{4+}$$_4$$O_{9}$$.$3.85$H_2O$. The mineral has a hexagonal unit ceil with a=2.840 $\AA$ c=7.486 $\AA$ and a : c = 1 : 2.636. The DTA curve shows endothermic peaks at 65, 180, 690 and 102$0^{\circ}C$. The IR absorption spectrum shows absorption bands at 445, 500, 1630 and 3400 c $m^{1}$. The mineral name Chimooite has been named in honour of late Prof, Chi Moo Son of Seoul National University.ity.versity.ity.y.
We prepared 10cm-diameter Si(100)/500 $\AA$-Si$_3$N$_4$/Si(100) wafer Pairs adopting 500 $\AA$ -thick Si$_3$N$_4$layer as insulating layer between single crystal Si wafers. Si3N, is superior to conventional SiO$_2$ in insulating. We premated a p-type(100) Si wafer and 500 $\AA$ -thick LPCVD Si$_3$N$_4$∥Si (100) wafer in a class 100 clean room. The cremated wafers are separated in two groups. One group is treated to have hydrophobic surface and the other to have hydrophilic. We employed a FLA(fast linear annealing) bonder to enhance the bond strength of cremated wafers at the scan velocity of 0.1mm/sec with varying the heat input at the range of 400~1125W. We measured bonded area using a infrared camera and bonding strength by the razor blade crack opening method. We used high resolution transmission electron microscopy(HRTEM) to probe cross sectional view of bonded wafers. The bonded area of two groups was about 75%. The bonding strength of samples which have hydrophobic surface increased with heat input up to 1577mJ/$m^2$ However, bonding strength of samples which have hydrophilic surface was above 2000mJ/$m^2$regardless of heat input. The HRTEM results showed that the hydrophilic samples have about 25 $\AA$ -thick SiO layer between Si and Si$_3$N$_4$/Si and that maybe lead to increase of bonding strength.
The maturity of amber matrix and inclusion was studied to explore the effect of heat treatment on the formation of the sun spangle in the transparent Baltic amber from Gdansk, Poland. Optical microscope revealed two types of inclusions in the original amber samples. The inclusions in the amber which had sun spangle were dramatically expanded by the heat treatment, comparing to those without sun spangle which contains fissure and shows different refractive index. The amber sample which didn't show sun spangle after the heat treatment showed a strong carbon related peak in TOF-SIMS spectra and weak oxygen related peak. it means that the maturity of this amber sample is comparatively higher than the one with spangle. The two amber samples show similar IR spectra before the heat treatment. However, the amber which had sun spangle exhibited an additional 1019 $cm^{-1}$ absorption peak and a more intense 887 $cm^{-1}$ peak. The different chemical compositions between the two types of amber is believed to be due to the different absorption spectra between 1000~600 $cm^{-1}$. According to the study of DSC analysis, the two samples show different DSC profiles. Although they have the same geological origin, their geological ages are different and have different chemical compositions. Thus, they exhibited different behavior after the heat treatment. The formation of sun spangle seemed to depend on the difference in the heat expansion rate of amber matrix with different maturity and chemical compositions.
Lee, Seon Yong;Choi, Su-Yeon;Chang, Bongsu;Lee, Young Jae
Korean Journal of Mineralogy and Petrology
/
v.35
no.2
/
pp.111-123
/
2022
Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO32-) and sulfate (SO42-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.
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