• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.355.1-355.1
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• 2014

Zirconium nitride (ZrN)는 높은 녹는점과 기계적 강도 그리고 내식성을 가져 부품 산업계에서 hard coating에 이용된다. 또한 금속과 같은 전기 전도성을 가지므로 초고집적소자의 확산방지막에 이르기까지 많은 응용이 되고 있다. 본 실험에서는 Si 기판 위에rf magnetron sputter를 사용하여 Zr박막을 증착 하였으며 질소 유량을 변화시키며 Zirconium nitride 박막을 증착하였다. 증착된 박막의 질소 유량변화에 따른 nano-electrotribology 특성변화를 관찰하기 위해 nano-indenter를 사용하였다. 또한 Weibull statistics을 사용하여 박막의 균일성을 검증하였다. 질소 유량이 각각 0, 0.5, 5 sccm으로 증가하는 동안 surface hardness는 12.37, 10.49, 12.14 GPa로 변화하였다. 이때, 박막의 elastic modulus는 175.27, 163.94, 172.18 GPa로 각각 변화하였다. 이러한 결과는 질소 유량에 따라zirconium nitride가 여러 상으로 생성되는 것으로 해석할 수 있다.

• Proceedings of the Materials Research Society of Korea Conference
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• 2012.05a
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• pp.102.2-102.2
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• 2012

Different layers of zirconium nitride (ZrN) and hydroxyapatite (HA) coatings were prepared on cp Ti substrate for biomedical applications. The main idea is to improve the mechanical strength as well as the biocompatibility of the coating. ZrN is known for its high mechanical strength, corrosion resistance. HA is well known for its biocompatibility properties. Hence, in this study, both materials were coated on a cp Ti substrate with bottom layer with ZrN for good bonding with substrate and the top layer with HA for induce bioactivity. Middle layer was formed by a composite of HA and ZrN. Detail analyses of the layered coatings for its structural, morphological, topographical properties were carried out. Then the mechanical property of the layered coatings was analyzed by nanoindentation. Biomimetic growths of apatite on the functionally graded coatings were determined by simulated body fluid method. This study provides promising results to use this kind of coatings in biomedical field.

• Journal of Dental Rehabilitation and Applied Science
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• v.32 no.3
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• pp.194-201
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• 2016

Purpose: The purpose of this study was to evaluate of Zirconium Nitride (ZrN) coating on shear bond strength with denture base resin in Co-Cr and Ti-6Al-4V alloy. Materials and Methods: Co-Cr and Ti-6Al-4V alloy disks (10 mm in diameter, 2.5 mm in thickness; each other: n = 14) were prepared and divided with 2 groups each other by ZrN coating. After primer was applied to disks surface, denture base resin with diameter 6 mm, height 5 mm was bonded on metal disk surface. After surface roughness was measured by Profiler, shear bond strength was determined with Universal testing machine and analyzed with two-way ANOVA. The specimen surfaces and failure mode were examined using a scanning electron microscope. Results: ZrN coated groups showed significantly higher rough surface than non-coated groups (P < 0.05). Irrespective of alloy materials, shear bond strength of ZrN coated groups were lower than non-coated groups (P < 0.001). The scanning electron microscope (SEM) of ZrN coated groups showed mixed and adhesive fractures. Conclusion: ZrN coating weakened bonding strength between denture base resin and Co-Cr, Ti-6Al-4V alloy.

• The Journal of Advanced Prosthodontics
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• v.7 no.2
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• pp.166-171
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• 2015

PURPOSE. The aim of this study was to evaluate antibacterial activity and osteoblast-like cell viability according to the ratio of titanium nitride and zirconium nitride coating on commercially pure titanium using an arc ion plating system. MATERIALS AND METHODS. Polished titanium surfaces were used as controls. Surface topography was observed by scanning electron microscopy, and surface roughness was measured using a two-dimensional contact stylus profilometer. Antibacterial activity was evaluated against Streptococcus mutans and Porphyromonas gingivalis with the colony-forming unit assay. Cell compatibility, mRNA expression, and morphology related to human osteoblast-like cells (MG-63) on the coated specimens were determined by the XTT assay and reverse transcriptase-polymerase chain reaction. RESULTS. The number of S. mutans colonies on the TiN, ZrN and $(Ti_{1-x}Zr_x)N$ coated surface decreased significantly compared to those on the non-coated titanium surface (P<0.05). CONCLUSION. The number of P. gingivalis colonies on all surfaces showed no significant differences. TiN, ZrN and $(Ti_{1-x}Zr_x)N$ coated titanium showed antibacterial activity against S. mutans related to initial biofilm formation but not P. gingivalis associated with advanced periimplantitis, and did not influence osteoblast-like cell viability.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.355.2-355.2
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• 2014

Zirconium nitride (ZrN)는 높은 열적, 화학적 특성과 우수한 기계적 강도, 낮은 전기 저항성 때문에 절삭공구, 의료용품 등으로 널리 사용된다. 특히 물리증착법 (PVD)으로 증착 할 경우 실제 hardness보다 높은 특성을 가지고 내마모성과 고온에서 hardness가 우수한 것으로 알려져 있다. 본 실험에서는 물리증착법 중 하나인 rf magnetron sputter를 사용하여 질소 유량에 따른 zirconium nitride 박막을 증착하였다. 그 후, $600^{\circ}C$, N2 분위기에서 후열처리를 진행하였고, 후열처리에 따른 박막의 nano-electrotribology 특성 변화를 관찰하기 위해 nano-indenter를 사용하였다. 측정결과, 질소 유량이 0, 0.5, 5 sccm으로 변함에 따라 증착된 박막의 hardness는 18.62, 15.64, 13.58 GPa로 각각 감소되었으며, elastic moduls도 210.43, 185.15, 171.52 GPa로 감소하였다. 이는 증착 과정에서 과포화된 N2 가 후열처리 과정에서 빠져 나오는 것으로 알 수 있다.

• Bulletin of the Korean Chemical Society
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• v.28 no.10
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• pp.1751-1755
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• 2007

The interaction of ammonium hydroxide (NH4OH) with zircaloy-4 (Zry-4) was investigated using X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) methods. In order to study the surface chemistry of NH4OH/Zry-4 system, the binding energies of N1s, O1s and Zr3d electrons were monitored. The N1s peak intensity was remarkably increased by following cycles of Ar+ sputtering of NH4OH dosed Zry-4 surface at room temperature. Because the nitrogen stayed under the subsurface region was diffused out onto the Zry-4 surface after oxygen concentration was decreased. These could be occurred after the surface oxygen was diffused into the bulk or desorbed out from the surface until Ar+ fluence was 6.0 × 1016 Ar+/cm2 then the surface was relatively atomic deficient state. The O1s peak intensity was decreased by stepwise Ar+ sputtering. After many cycles of Ar+ sputtering, the peak intensities of Zr3d peaks did not change much but the shape of the peak clearly did change. This implies that the oxidation state of zirconium was changed during stepwise Ar+ sputtering of NH4OH/Zry-4. The Zr3d peak intensity of zirconium nitride (ZrNx) increased as the intensity of N1s (from zirconium nitride) increased but the Zr3d peak intensity of zirconium oxide (ZrOx) decreased due to the depopulation of the oxygen species on the surface region. We also observed that the peak intensity of Zr4+ was nearly same after Ar+ sputtering processes but the peak intensity of metallic zirconium increased compared to that of before the sputtering process was performed.

• Journal of the Korean Ceramic Society
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• v.25 no.2
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• pp.184-190
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• 1988

ZrN powder was prepared from the powder mixture of ZrCl4 and Al by the halogenide process in nitrogen gas flow (100-150ml/min) at the temperatures from 200$^{\circ}$to 1050$^{\circ}C$. ZrN powder was formed about 600$^{\circ}C$ and in the slow nitriding reaction, however, an intermediate product of Al3Zr was formed. The fine powder (0.1-10$\mu\textrm{m}$) of single phase ZrN was obtained at 1050$^{\circ}C$ after 1 hour. The lattice parameter and crystallite size of ZrN were 4.5787A and 360A, respectively. According to SEM observation, the particles were apt to agglomerates. The apparent activation energy for the formation of ZrN was approximately 13.2kcal/mole(750$^{\circ}$-1000$^{\circ}C$).

• Journal of the Korean Applied Science and Technology
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• v.20 no.4
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• pp.358-365
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• 2003

Zirconium nitride powders were synthesized at a relatively lower temperature using methane as a reducing agent in the nitridation of zircoia. $ZrO_2$ powder was prepared by a sol-gel technique. The resulting sol-gel was centrifuged, and the gel was washed with deionized water. Anhydrous ammonia was used as the nitrogen source and methane was used as the reducing agent. Conversion diagrams show the equilibrium solid phase as a function of reagent concentrations for a specific temperature and gas pressure for the reagent system $NH_3-ZrO_2-CH_4$. The reagent concentration ranges within which pure ZrN is formed increase with increasing reaction temperature. Low pressure with an excess of hydrogen decreases the reaction temperature at which pure ZrN is formed. Low pressure together with the introduction of excess hydrogen into the reaction system increases Zr and N conversion efficiency and retards C deposition.

• Korean Journal of Materials Research
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• v.22 no.5
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• pp.243-248
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• 2012

ZrN nanoparticles were prepared by an exothermic reduction of $ZrCl_4$ with $NaN_3$ in the presence of NaCl flux in a nitrogen atmosphere. Using a solid-state combustion approach, we have demonstrated that the zirconium nitride nanoparticles synthesis process can be completed in only several minutes compared with a few hours for previous synthesis approaches. The chemistry of the combustion process is not complex and is based on a metathesis reaction between $ZrCl_4$ and $NaN_3$. Because of the low melting and boiling points of the raw materials it was possible to synthesize the ZrN phase at low combustion temperatures. It was shown that the combustion temperature and the size of the particles can be readily controlled by tuning the concentration of the NaCl flux. The results show that an increase in the NaCl concentration (from 2 to 13 M) results in a temperature decrease from 1280 to $750^{\circ}C$. ZrN nanoparticles have a high surface area (50-70 $m^2/g$), narrow pore size distribution, and nano-particle size between 10 and 30 nm. The activation energy, which can be extracted from the experimental combustion temperature data, is: E = 20 kcal/mol. The method reported here is self-sustaining, rapid, and can be scaled up for a large scale production of a transition metal nitride nanoparticle system (TiN, TaN, HfN, etc.) with suitable halide salts and alkali metal azide.

• The Journal of Korean Academy of Prosthodontics
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• v.44 no.6
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• pp.740-750
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• 2006

Statement of problems. In an attempt to reduce screw loosening, dry lubricant coatings such as pure gold or tefron have been applied to the abutment screw. However, under repeated tightening and loosening procedures, low wear resistance and adhesion strength of coating material produced free particles on the surface of abutment screw and increased frictional resistance resulting in screw tightening problems. Purpose. The aim of this study was to compare friction coefficient, adhesion strength, vickers hardness and evaluate coating surface of titanium alloy specimens coated with TiN(titanium nitride), ZrN(zirconium nitride) and WC(tungsten carbide). Material and method. Titanium alloy(Ti-6Al-4V) discs of 12mm in diameter and 1mm in thickness divided into 4 groups. TiN, ZrN and WC was coated for the specimens of 3 groups respectively, and those of 1 group were not coated. Each group was made up of 4 specimens. In this study, sputtering method was used among the PVD(Physical Vapor Deposition) techniques available for TiN, ZrN and WC coatings. Friction coefficient, adhesion strength, vickers hardness and coating surface of 4 groups were measured. Results. 1. For all three coating conditions, friction coefficient was significantly decreased. Especially, ZrN coated surface showed the lowest value. $TiN(0.39{\pm}0.02)$, $ZrN(0.24{\pm}0.01)$, $WC(0.31{\pm}0.03)$. 2. TiN coating showed the highest adhesion strength, however ZrN coating had the lowest value. $TiN(25.3N{\pm}1.6)$, $ZrN(14.8N{\pm}0.6)$, $ WC(18.4N{\pm}0.7)$. 3. Vickers hardness of all three coatings was remarkably increased as compared with that of none coated specimen. TiN coating had the highest Vickers hardness, however WC coating showed the lowest value. $TiN(1865.2{\pm}33.8)$, $ZrN(1814.4{\pm}18.6)$, $WC(1008.5{\pm}35.9)$. 4. The ZrN or WC coated specimen showed a homogeneous and smooth surface, however the rough surface with defects was observed for TiN coating. Conclusions. When TiN, ZrN and WC coating applied to the abutment screw, frictional resistance would be reduced, as a result, the greater preload and prevention of the screw loosening could be expected.