• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2000.11a
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• pp.3-4
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• 2000

Many researchers are interested in the synthesis and characterization of carbon nitride and diamond-like carbon (DLq because they show excellent mechanical properties such as low friction and high wear resistance and excellent electrical properties such as controllable electical resistivity and good field electron emission. We have deposited amorphous carbon nitride (a-C:N) thin films and DLC thin films by shielded arc ion plating (SAIP) and evaluated the structural and tribological properties. The application of appropriate negative bias on substrates is effective to increase the film hardness and wear resistance. This paper reports on the deposition and tribological OLC films in relation to the substrate bias voltage (Vs). films are compared with those of the OLC films. A high purity sintered graphite target was mounted on a cathode as a carbon source. Nitrogen or argon was introduced into a deposition chamber through each mass flow controller. After the initiation of an arc plasma at 60 A and 1 Pa, the target surface was heated and evaporated by the plasma. Carbon atoms and clusters evaporated from the target were ionized partially and reacted with activated nitrogen species, and a carbon nitride film was deposited onto a Si (100) substrate when we used nitrogen as a reactant gas. The surface of the growing film also reacted with activated nitrogen species. Carbon macropartic1es (0.1 -100 maicro-m) evaporated from the target at the same time were not ionized and did not react fully with nitrogen species. These macroparticles interfered with the formation of the carbon nitride film. Therefore we set a shielding plate made of stainless steel between the target and the substrate to trap the macropartic1es. This shielding method is very effective to prepare smooth a-CN films. We, therefore, call this method "shielded arc ion plating (SAIP)". For the deposition of DLC films we used argon instead of nitrogen. Films of about 150 nm in thickness were deposited onto Si substrates. Their structures, chemical compositions and chemical bonding states were analyzed by using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and infrared spectroscopy. Hardness of the films was measured with a nanointender interfaced with an atomic force microscope (AFM). A Berkovich-type diamond tip whose radius was less than 100 nm was used for the measurement. A force-displacement curve of each film was measured at a peak load force of 250 maicro-N. Load, hold and unload times for each indentation were 2.5, 0 and 2.5 s, respectively. Hardness of each film was determined from five force-displacement curves. Wear resistance of the films was analyzed as follows. First, each film surface was scanned with the diamond tip at a constant load force of 20 maicro-N. The tip scanning was repeated 30 times in a 1 urn-square region with 512 lines at a scanning rate of 2 um/ s. After this tip-scanning, the film surface was observed in the AFM mode at a constant force of 5 maicro-N with the same Berkovich-type tip. The hardness of a-CN films was less dependent on Vs. The hardness of the film deposited at Vs=O V in a nitrogen plasma was about 10 GPa and almost similar to that of Si. It slightly increased to 12 - 15 GPa when a bias voltage of -100 - -500 V was applied to the substrate with showing its maximum at Vs=-300 V. The film deposited at Vs=O V was least wear resistant which was consistent with its lowest hardness. The biased films became more wear resistant. Particularly the film deposited at Vs=-300 V showed remarkable wear resistance. Its wear depth was too shallow to be measured with AFM. On the other hand, the DLC film, deposited at Vs=-l00 V in an argon plasma, whose hardness was 35 GPa was obviously worn under the same wear test conditions. The a-C:N films show higher wear resistance than DLC films and are useful for wear resistant coatings on various mechanical and electronic parts.nic parts.

• Journal of the Mineralogical Society of Korea
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• v.5 no.2
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• pp.109-121
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• 1992

For the purpose of mineralogical and chemical study on the topazes from various localities of world(Brzail, China, India, Nigeria and Sri Lanka), electron microprobe analysis(EPMA), neutron activation analysis(NAA), X-ray diffractometry, Raman spectroscopy, etch test, scanning electron microscopy, refractive index, specific gravity, fluid inclusion were performed. The chemical composition in topaz was discussed along with its physical and structural properties. Variations in the unit-cell dimension and physical properties of topaz were found to have a close relations in the unit-cell dimension and physical properties of topaz were found to have a close relationship with extent of substitution of $OH^-\;for\;F^-$. According to neutron activation analyses, the trace elements had no effects on the physical properties of topaz. Raman spectra showed that the peaks of topaz were different in intensity from one locality to another. Etching defects in topaz includes negative crystal defect o point-bottom pit(India, Nigeria) and net work defect of curl-bottom pit(Brazil, China). Fluid inclusions in topaz may be classiffied into liquid $CO_2$-bearing inclusion, gaseous inclusion, halite, sylvite-bearing inclusion and liquid inclusion. The results of this study can be useful to devising artificial coloring methods for topaz with different mineralogical compositions.

• Journal of the Korean Ceramic Society
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• v.39 no.9
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• pp.863-870
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• 2002

The Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$ (x=0.0∼1.0) solid solutions were successfully synthesized and their ordering structures as well as dielectric properties were investigated ${{r(Nb^{5+})=r(Ta^{5+})=0.78 {\AA},\;AW(Nb^{5+})=92.91,\;AW(Ta^{5+})=180.95}}$. While $Pb(Fe_{1/2}Ta_{1/2})O_3$ showed typical relaxor ferroelectric characteristics such as dielectric relaxation and diffuse phase transition, the sharpeness of the phase transition increased as $Ta^{5+}$ was replaced by $Nb^{5+}$ and finally $Pb(Fe_{1/2}Nb_{1/2})O_3$ showed normal ferroelectric characteristics with no dielectric relaxation. By using Raman spectroscopy, it was revealed that the $Fe^{3+}\;and\;Ta^{5+}\;of\;Pb(Fe_{1/2}Ta_{1/2})O_3$ were stoichiometrically 1:1 ordered within the short range which can be hardly probed even by TEM. Also, The degree of ordering in $Pb(Fe_{1/2}Ta_{1/2})O_3$ decreased as $Ta^{5+}$ was replaced by $Nb^{5+}$ and finally $Fe^{3+}\;and\;Nb^{5+}\;of\;Pb(Fe_{1/2}Nb_{1/2})O_3$ were completely disordered. The relaxor ferroelectric characteristics of $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the stoichiometric 1:1 ordering of B-site cations within the short range which can be hardly probed even by TEM. Also, the decrease of the relaxor ferroelectric characteristics with the replacement of $Ta^{5+}\;by\;Nb^{5+}$ could be correlated with the weakening of the ordering and the normal ferroelectric characteristics of $Pb(Fe_{1/2}Nb_{1/2})O_3$ could be correlated with the complete disordering of B-site cations.

• Bulletin of the Korean Chemical Society
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• v.24 no.4
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• pp.446-452
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• 2003

Some new nanohybrid materials have been synthesized by intercalating the oxotitanium(IV) meso-tetrakis(4- sulfonatophenyl) porphyrin$(O=Ti^{(IV)} TSPP)$ into the Zn/Al layered double hydroxides (LDHs), and their structures and photophysical properties have been investigated by various laser spectroscopic techniques. According to the XRD pattern of the synthesized nanohybrid materials, the macrocycle plane of $O=Ti^{(IV)}$ TSPP are grafted perpendicular to the LDH layers. The $O=Ti^{(IV)}$ TSPP-intercalated LDH exhibits band broadening of the absorption spectrum and a blue shift of Q-band as compared to that observed in solution. Resonance Raman spectral measurements demonstrate that the positively charged LDHs give rise to a slight decrease of the electronic density of the porphyrin ring accompanying a small change of the electronic distribution of the $O=Ti^{(IV)}$ TSPP. Consequently the LDH environment affects the energies of the two highest occupied molecular orbitals (HOMOs) of the $O=Ti^{(IV)}$) TSPP, $a_{1u}$ and $a_{2u}$, producing a mixed orbital character. Being consistent with these electronic structural changes of $O=Ti^{(IV)}$ TSPP in LDH, both the fluorescence spectral change and the fsdiffuse reflectance transient measurements imply that the photoexcitation of the $O=Ti^{(IV)}$ TSPP intercalated into LDH undergoes fast relaxation to the O=Ti(IV) $TSPP^+-LDH^- $charge transfer (CT) state within a few picoseconds, followed by a photoinduced electron transfer between the O=Ti(IV) TSPP and LDHs with a rate constant greater than %1×10^{10}S^{-1}$. No evidence is found for back electron transfer. In conclusion, the $O=Ti^{(IV)}$ TSPP intercalated LDH seems to be a possible candidate for an artificial reaction center for an efficient solar energy conversion system.

• Applied Chemistry for Engineering
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• v.8 no.5
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• pp.742-748
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• 1997

Diamond films which have high hardness and thermal conductivity can be used to improve the performance of WC-Co as a cutting tool material. However, it is difficult to get such coatings of good uniformity and adhesiveness due to the surface characteristics of WC-Co. To get better coatings, some techniques, such as the surface treatment of substrate or the formation of interlayer between substrate and diamond film, have been tried. In the present work, the nickel interlayer is formed onto WC-Co by electroless Ni-P plating, which is introduced as a new method, and then diamond film is deposited on the interlayer. Formation and uniformity of three layers, i.e., substrate, electroless plate, and diamond film, and the adhesiveness of interlayers were studied. To investigate the effects of pretreatment on electroless plating, two different methods such as acid treatment and diamond powder treatment were used. The effects of heat treatment of the electroless plated surface on adhesiveness between the substrate and the interlayer were examined. It was found that as the temperature increases, the Ni crystals grow and then result in improved adhesiveness. Diamond film coatings of pure diamond phase were obtained at $800^{\circ}C$. It is concluded that the heat treated electroless Ni-P plating can be effectively used as a interlayer between WC-Co substrate and diamond film.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.412-412
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• 2009

Carbon-based nano materials have a significant effect on various fields such as physics, chemistry and material science. Therefore carbon nano materials have been investigated by many scientists and engineers. Especially, since graphene, 2-dimemsonal carbon nanostructure, was experimentally discovered graphene has been tremendously attracted by both theoretical and experimental groups due to their extraordinary electrical, chemical and mechanical properties. Electrical conductivity of graphene is about ten times to that of silicon-based material and independent of temperature. At the same time silicon-based semiconductors encountered to limitation in size reduction, graphene is a strong candidate substituting for silicon-based semiconductor. But there are many limitations on fabricating large-scale graphene sheets (GS) without any defect and controlling chirality of edges. Many scientists applied micromechanical cleavage method from graphite and a SiC decomposition method to the fabrication of GS. However these methods are on the basic stage and have many drawbacks. Thereupon, our group fabricated GS through Thermo-electrical Pulse Induced Evaporation (TPIE) motivated by arc-discharge and field ion microscopy. This method is based on interaction of electrical pulse evaporation and thermal evaporation and is useful to produce not only graphene but also various carbon-based nanostructures with feeble pulse and at low temperature. On fabricating GS procedure, we could recognize distinguishable conditions (electrical pulse, temperature, etc.) to form a variety of carbon nanostructures. In this presentation, we will show the structural properties of OS by synthesized TPIE. Transmission Electron Microscopy (TEM) and Optical Microscopy (OM) observations were performed to view structural characteristics such as crystallinity. Moreover, we confirmed number of layers of GS by Atomic Force Microscopy (AFM) and Raman spectroscopy. Also, we used a probe station, in order to measure the electrical properties such as sheet resistance, resistivity, mobility of OS. We believe our method (TPIE) is a powerful bottom-up approach to synthesize and modify carbon-based nanostructures.

• 한국신재생에너지학회:학술대회논문집
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• 2005.11a
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• pp.561-566
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• 2005

Polycrystalline silicon films were deposited using hot wire CVD (HWCVD). The deposition of silicon thin films was approached by the theory of charged clusters (TCC). The TCC states that thin films grow by self-assembly of charged clusters or nanoparticles that have nucleated in the gas phase during the normal thin film process. Negatively charged clusters of a few nanometer in size were captured on a transmission electron microscopy (TEM) grid and observed by TEM. The negatively charged clusters are believed to have been generated by ion-induced nucleation on negative ions, which are produced by negative surface ionization on a tungsten hot wire. The electric current on the substrate carried by the negatively charged clusters during deposition was measured to be approximately $-2{\mu}A/cm^2$. Silicon thin films were deposited at different $SiH_4$ and $H_2$ gas mixtures and filament temperatures. The crystalline volume fraction, grain size and the growth rate of the films were measured by Raman spectroscopy, X-ray diffraction and scanning electron microscopy. The deposit ion behavior of the si1icon thin films was related to properties of the charged clusters, which were in turn controlled by the process conditions. In order to verify the effect of the charged clusters on the growth behavior, three different electric biases of -200 V, 0 V and +25 V were applied to the substrate during the process, The deposition rate at an applied bias of +25 V was greater than that at 0 V and -200 V, which means that the si1icon film deposition was the result of the deposit ion of charged clusters generated in the gas phase. The working pressures had a large effect on the growth rate dependency on the bias appled to the substrate, which indicates that pressure affects the charging ratio of neutral to negatively charged clusters. These results suggest that polycrystalline silicon thin films with high crystalline volume fraction and large grain size can be produced by control1ing the behavior of the charged clusters generated in the gas phase of a normal HWCVD reactor.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.642-642
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• 2013

Graphene, two dimensional single layer of carbon atoms, has tremendous attention due to its superior property such as high electron mobility, high thermal conductivity and optical transparency. Especially, chemical vapor deposition (CVD) grown graphene has been used as a promising material for high quality and large-scale graphene film. Unfortunately, although CVD-grown graphene has strong advantages, application of the CVD-grown graphene is limited due to ineffective transfer process that delivers the graphene onto a desired substrate by using polymer support layer such as PMMA(polymethyl methacrylate). The transferred CVD-grown graphene has serious drawback due to remaining polymeric residues generated during transfer process, which induces the poor physical and electrical characteristics by a p-doping effect and impurity scattering. To solve such issue incurred during polymer transfer process of CVD-grown graphene, various approaches including thermal annealing, chemical cleaning, mechanical cleaning have been tried but were not successful in getting rid of polymeric residues. On the other hand, lithographical patterning of graphene is an essential step in any form of microelectronic processing and most of conventional lithographic techniques employ photoresist for the definition of graphene patterns on substrates. But, application of photoresist is undesirable because of the presence of residual polymers that contaminate the graphene surface consistent with the effects generated during transfer process. Therefore, in order to fully utilize the excellent properties of CVD-grown graphene, new approach of transfer and patterning techniques which can avoid polymeric residue problem needs to be developed. In this work, we carried out transfer and patterning process simultaneously with no polymeric residue by using a metal etch mask. The patterned thin gold layer was deposited on CVD-grown graphene instead of photoresists in order to make much cleaner and smoother surface and then transferred onto a desired substrate with PMMA, which does not directly contact with graphene surface. We compare the surface properties and patterning morphology of graphene by scanning electron microscopy (SEM), atomic force microscopy(AFM) and Raman spectroscopy. Comparison with the effect of residual polymer and metal on performance of graphene FET will be discussed.

• Journal of Conservation Science
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• v.36 no.3
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• pp.162-177
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• 2020

Research was conducted to characterize the copper production and smelting process with 11 copper smelting by-products (copper slag and copper crucible) excavated from the NA and LA areas at the Gwanbuk-ri archeological site in Buyeo. Scanning electron microscopy-energy dispersive spectroscopy, wavelength dispersive X-ray fluorescence, X-ray diffraction, and Raman microspectroscopy were employed in the analysis. The research results reveal that the copper slag from Gwanbuk-ri contained silicate oxide, magnetite, fayalite, and delafossite, which are typical characteristics of crucible slag and refined slag. The outward appearance and microstructure of the slag were grouped as follows: 1. glassy matrix + Cu prill, 2. glassy matrix + Cu prill + magnetite, 3. silicate mineral matrix + Cu prill, 4. crystalline (delafossite and magnetite) + amorphous (Cu prill), 5. magnetite + fayalite, and 6. slag from slag. The copper slags from Guanbuk-ri were found to contain residues of impurities such as SiO₂, Al₂O₃, CaO, SO₄, P₂O₅, Ag₂O, and Sb₂O₃ in their microstructure, and, in some cases, it was confirmed that copper, tin and lead are alloys. These results indicate that refining of intermediate copper(including impurities) and refining of alloys of copper(including impurities) - tin and refining of copper(including impurities) - tin - lead took place during the copper production process at Gwanbuk-ri, Buyeo.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.58-58
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• 1999

The diamond films which can be applied to SOD (silicon-on-diamond) structure were deposited on Si(100) substrate using CO/H2 CH4/H2 source gases by microwave plasma chemical vapor deposition(MPCVD), and SOD structure have been fabricated by poly-silicon film deposited on the diamond/Si(100) structure y low pressure chemical vapor deposition(LPCVD). The phase of the diamond film, surface morpholog, and diamond/Si(100) interface were confirmed by X-ray diffraction(XRD), scanning electron microscopy(SEM), atomic force microscopy(AFM), and Raman spectroscopy. The dielectric constant, leakage current and resistivity as a function of temperature in films are investigated by C-V and I-V characteristics and four-point probe method. The high quality diamond films without amorphous carbon and non-diamond elements were formed on a Si(100), which could be obtained by CO/H2 and CH4/H2 concentration ratio of 15.3% and 1.5%, respectively. The (111) plane of diamond films was preferentially grown on the Si(100) substrate. The grain size of the films deposited by CO/H2 are gradually increased from 26nm to 36 nm as deposition times increased. The well developed cubo-octahedron 100 structure nd triangle shape 111 are mixed together and make smooth and even film surface. The surface roughness of the diamond films deposited by under the condition of CO/H2 and CH4/H2 concentration ratio of 15.3% and 1.5% were 1.86nm and 3.7 nm, respectively, and the diamond/Si(100) interface was uniform resistivity of the films deposited by CO/H2 concentration ratio of 15.3% are obtained 5.3, 1$\times$10-9 A/cm, 1 MV/cm2, and 7.2$\times$106 $\Omega$cm, respectively. In the case of the films deposited by CH4/H2 resistivity are 5.8, 1$\times$10-9 A/cm, 1 MV/cm, and 8.5$\times$106 $\Omega$cm, respectively. In this study, it is known that the diamond films deposited by using CO/H2 gas mixture as a carbon source are better thane these of CH4/H2 one.