• Journal of Electrical Engineering and Technology
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• v.4 no.4
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• pp.538-545
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• 2009

The SiC-$ZrB_2$ composites were fabricated by combining 30, 35, 40 and 45vol.% of Zirconium Diboride (hereafter, $ZrB_2$) powders with Silicon Carbide (hereafter, SiC) matrix. The SiC-$ZrB_2$ composites, the sintered compacts, were produced through Spark Plasma Sintering (hereafter, SPS), and its physical, electrical, and mechanical properties were examined. Also, the thermal image analysis of the SiC-$ZrB_2$ composites was examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed via X-Ray Diffractometer (hereafter, XRD) analysis. The relative density of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$, and SiC+45vol.%$ZrB_2$ composites were 88.64%, 76.80%, 79.09% and 88.12%, respectively. The XRD phase analysis of the sintered compacts demonstrated high phase of SiC and $ZrB_2$ but low phase of $ZrO_2$. Among the SiC-$ZrB_2$ composites, the SiC+35vol.%$ZrB_2$ composite had the lowest flexural strength, 148.49MPa, and the SiC+40vol.%$ZrB_2$ composite had the highest flexural strength, 204.85MPa, at room temperature. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$, SiC+40vol.%$ZrB_2$ and SiC+45vol.%$ZrB_2$ composites were $6.74\times10^{-4}$, $4.56\times10^{-3}$, $1.92\times10^{-3}$, and $4.95\times10^{-3}\Omega{\cdot}cm$ at room temperature, respectively. The electrical resistivities of the SiC+30vol.%$ZrB_2$, SiC+35vol.%$ZrB_2$ SiC+40vol.%$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites had Positive Temperature Coefficient Resistance (hereafter, PTCR) in the temperature range from $25^{\circ}C$ to $500^{\circ}C$. The V-I characteristics of the SiC+40vol.%$ZrB_2$ composite had a linear shape. Therefore, it is considered that the SiC+40vol.%$ZrB_2$ composite containing the most outstanding mechanical properties, high resistance temperature coefficient and PTCR characteristics among the sintered compacts can be used as an energy friendly ceramic heater or electrode material through SPS.

• Proceedings of the KIEE Conference
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• 2009.07a
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• pp.1252_1253
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• 2009

The composites were fabricated by adding 0, 15, 20, 25[vol.%] Zirconium Diboride(hereafter, $ZrB_2$) powders as a second phase to Silicon Carbide(hereafter, SiC) matrix. The physical, mechanical and electrical properties of electroconductive SiC ceramic composites by spark plasma sintering(hereafter, SPS) were examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed in the XRD analysis The relative density of mono SiC, SiC+15[vol.%]$ZrB_2$, SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ composites are 90.97[%], 74.62[%], 77.99[%] and 72.61[%] respectively. The XRD phase analysis of the electroconductive SiC ceramic composites reveals high of SiC and $ZrB_2$ and low of ZrO2 phase. The electrical resistivity of mono SiC, SiC+15[vol.%]$ZrB_2$, SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ composites are $4.57{\times}10^{-1}$, $2.13{\times}10^{-1}$, $1.53{\times}10^{-1}$ and $6.37{\times}10^{-2}[{\Omega}{\cdot}cm]$ at room temperature, respectively. The electrical resistivity of mono SiC, SiC+15[vol.%]$ZrB_2$, SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ are Negative Temperature Coefficient Resistance(hereafter, NTCR) in temperature ranges from 25[$^{\circ}C$] to 100[$^{\circ}C$]. It is convinced that SiC+20[vol.%]$ZrB_2$ composite by SPS can be applied for heater above 1000[$^{\circ}C$].

• Korean Journal of Materials Research
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• v.7 no.11
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• pp.964-968
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• 1997

Si(001)기판 위에 형성시킨 Zr-silicide의 전기적, 물리적 특성에 관한 연구를 하였다. Zr 박막은 전자빔 증착기를 사용하여 증착하였으며, 50$0^{\circ}C$ 열처리하여 Zr-silicide를 형성시켰다. 각 온도에서 열처리된 Zr-silicide시편의 상형성, 전기적 특성, 화학적 조성, 표면 및 계면 형상을 XRD, four-point probe, AES, TEM과 HRTEM으로 분석하였다. 분석 결과 $600^{\circ}C$부터 Zr과 Si기판의 계면에서 C49 ZrSi$_{2}$의 생성이 관찰되었다. Zr-Silicide박막의 비저항은 C49 ZrSi$_{2}$의 형성에 영향을 받는 것으로 관찰되었으며, 50$0^{\circ}C$ 열처리 후에는 184.3 $\mu$Ω-cm로 낮아졌으며, C49 ZrSi$_{2}$가 박막에 완전히 형성된 80$0^{\circ}C$ 열처리 후에는 32$\mu$Ω-cm의 낮은 저항을 나타내었다. 형성된 C49 ZrSi$_{2}$박막은 균질한 화학적 조성을 하고 있음을 AES 분석으로 확인하였다. Zr-silicide의 표면 및 계면의 형상을 TEM과 HRTEM으로 관찰하였으며, $600^{\circ}C$ 열처리 후에 계면에서 ZrSi$_{2}$의 상형성이 시작되는 것을 관찰하였다. 80$0^{\circ}C$ 열처리 후에도 계면과 표면형상은 비교적 균질한 형상이 유지되었음이 관찰되었으며, 이는 C49 ZrSi$_{2}$가 높은 온도에서도 잘 응집되지 않으며 고온 안정성을 가지는 재료임이 관찰되었다.

• Journal of the Korean Ceramic Society
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• v.32 no.7
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• pp.853-857
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• 1995

ZrSiO4 powders were prepared from partially hydrolyzed solution of Si(OC2H5)4 and ZrOCl2.8H2O solution by the sol-gel method and formation rate of ZrSiO4 on the reaction parameter was investigated. In order to prepare homogeneous ZrSiO4 precursor gels, the H2O/Si(OC2H5)4 molar ratio of about 2, the pH of the ZrOCl2.8H2O solution fo about 4 and stirring time of the mixed solutions of about 2 hrs were appropriate. Formation of temperature of ZrSiO4 reduced about 15$0^{\circ}C$ by milling and formation of ZrSiO4 at 1300~135$0^{\circ}C$ showed an accelerative increase through the hedvall effect by silica.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1997.04a
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• pp.135-140
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• 1997

The influences of ZrB$_2$ additions to SiC on microstructural, DDM(Electrical Discharge Machining), mechanical and electrical properties were investigated. composites were prepared by adding 15, 30, 45 vol.% ZrB$_2$particles as a second phase to SiC matrix. SiC-ZrB$_2$ composites obtained by hot pressing for high temperature structural application were fully dense with the relative densities over 99%. The fracture toughness of the composites were increased with the ZrB$_2$contents. In case of composite containing 30vol.% ZrB$_2$, the flexural strength and fracture toughness showed 45% and 60% increase, respectively compared to that of monolithic SiC sample. The electrical resistivities of SiC-ZrB$_2$ composites decreased significantly with the ZrB$_2$ contents. The electrical resistivity of SiC-30vol.% ZrB$_2$ composite showed 6.50$\times$10$^{-4}$ $\Omega$.cm. Cutting velocity of EDM of SiC-ZrB$_2$ composites are directly proportional to duty factor of pulse width. Surface roughness, however, are not all proportional to pulse width. Higher-flexural strength composites show a trend toward smaller crater volumes, leaving a smoother surface; the average surface roughness of the SiC-ZrB$_2$ 15 vol.% composite with the flexural strengthe of 375㎫ was 3.2${\mu}{\textrm}{m}$, whereas the SiC-ZrB$_2$ 30.vol% composite of 457㎫ was 1.35${\mu}{\textrm}{m}$. In the SEM micrographs of the fracture surface of SiC-ZrB$_2$ composites, the SiC-ZrB$_2$ two phases are distinct; the white phase is the ZrB$_2$and the gray phase is the SiC matrix. In the SEM micrographs of the EDM surface, however, these phases are no longer distinct because of thicker recast layer of resolidified-melt-formation droplets present. It is shown that SiC-ZrB$_2$ composites are able to be machined without surface cracking.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.58 no.9
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• pp.1757-1763
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• 2009

The composites were fabricated by adding 0, 15, 20, 25[vol.%] Zirconium Diboride(hereafter, $ZrB_2$) powders as a second phase to Silicon Carbide(hereafter, SiC) matrix. The physical, mechanical and electrical properties of electroconductive SiC ceramic composites by Spark Plasma Sintering(hereafter, SPS) were examined. Reactions between ${\beta}-SiC$ and $ZrB_2$ were not observed in the XRD analysis. The relative density of mono SiC, SiC+15[vol.%]$ZrB_2$, SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ composites are 90.93[%], 74.62[%], 74.99[%] and 72.61[%], respectively. The XRD phase analysis of the electroconductive SiC ceramic composites reveals high of SiC and $ZrB_2$ and low of $ZrO_2$ phase. The lowest flexural strength, 108.79[MPa], shown in SiC+15[vol.%] $ZrB_2$ composite and the highest - 220.15[MPa] - in SiC+20[vol.%] $ZrB_2$composite at room temperature. The trend of the mechanical properties of the electroconductive SiC ceramic composites moves in accord with that of the relative density. The electrical resistivities of mono SiC, SiC+15[vol.%]$ZrB_2$, SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ composites are 4.57${\times}10^{-1}$, 2.13${\times}10^{-1}$, 1.53${\times}10^{-1}$ and 6.37${\times}10^{-2}$[${\Omega}$ cm] at room temperature, respectively. The electrical resistivity of mono SiC, SiC+15[vol.%]$ZrB_2$. SiC+20[vol.%]$ZrB_2$ and SiC+25[vol.%]$ZrB_2$ are Negative Temperature Coefficient Resistance(hereafter, NTCR) in temperature ranges from 25[$^{\circ}C$] to 100[$^{\circ}C$]. The declination of V-I characteristics of SiC+20[vol.%]$ZrB_2$ composite is 3.72${\times}10^{-1}$. It is convinced that SiC+20[vol.%]$ZrB_2$ composite by SPS can be applied for heater or electrode above 1000[$^{\circ}C$]

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.12 no.6
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• pp.283-287
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• 2002

We have studied Zr(Si)N film as a diffusion barrier between Cu metal and Si substrate for application of interconnection metal in ULSI circuits. Zr(Si)N film was deposited with reactive DC magnetron sputtering system using $Ar/N_2$mixed gas. The value of the resistivity was the lowest for the ZrN film using 29 : 1 of Ar : $N_2$reactant gas ratio at room temperature and decreased with increasing of Si substrate temperature. As the value of ZrN film resistivity was decreased, the direction of crystal growth was toward to (002) plane. The barrier property of ZrN film added with Si was improved. But Si was added too much in ZrN film, the barrier property was degraded. The adhesive property was improved with increasing of Si in ZrN. For the analysis of the film, XRD, Optical microscopy, Scretch tester, so on were used.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.58 no.4
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• pp.770-776
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• 2009

The composites were fabricated by adding 0, 15, 30, 45[vol.%] $ZrB_2$ powders as a second phase to SiC matrix. The physical, mechanical and electrical properties of electroconductive SiC ceramic composites by spark plasma sintering(SPS) were investigated. Reactions between ${\beta}$-SiC and $ZrB_2$ were not observed in the XRD and the phase analysis of the electroconductive SiC ceramic composites. The relative density of mono ${\beta}$-SiC, ${\beta}$-SiC+15[vol.%]$ZrB_2$, ${\beta}$-SiC+30[vol.%]$ZrB_2$ and ${\beta}$-SiC+45[vol.%]$ZrB_2$ composites are respectively 99.24[%], 87.53[%], 96.41[%] and 98.11[%] Phase analysis of the electroconductive SiC ceramic composites by XRD revealed mostly of ${\beta}$-SiC, $ZrB_2$ and weakly of $ZrO_2$ phase. The flexural strength showed the lowest of 114.44[MPa] for ${\beta}$-SiC+15[vol.%]$ZrB_2$ powders and showed the highest of 210.75[MPa] for composite no added with $ZrB_2$ powders at room temperature. The trend of the mechanical properties of the electroconductive SiC ceramic composites is accorded with the trend of the relative density. The electrical resistivity of the electroconductive SiC ceramic composites decreased with increased $ZrB_2$ contents. The electrical resistivity of mono ${\beta}$-SiC, ${\beta}$-SiC+15[vol.%]$ZrB_2$, ${\beta}$-SiC+30[vol.%]$ZrB_2$ and ${\beta}$-SiC+45[vol.%]$ZrB_2$ composites are respectively $4.57{\times}10^{-1},\;2.13{\times}10^{-1},\;2.68{\times}10^{-2}\;and\;1.99{\times}10^{-2}[{\Omega}{\cdot}cm]$ at room temperature. The electrical resistivity of mono ${\beta}$-SiC and ${\beta}$-SiC+15[vol.%]$ZrB_2$ are negative temperature coefficient resistance(NTCR) in temperature ranges from $25[^{\circ}C]\;to\; 100[^{\circ}C]$. The electrical resistivity of ${\beta}$-SiC+30[vol.%]$ZrB_2$ and ${\beta}$-SiC+45[vol.%]ZrB_2$ are positive temperature coefficient resistance(PTCR) in temperature ranges from $25[^{\circ}C]\;to\;100[^{\circ}C]$. It is convinced that ${\beta}$-SiC+30[vol.%]$ZrB_2$ composites by SPS for heater or ignitors can be applied.

• Proceedings of the KIEE Conference
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• 2009.07a
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• pp.1254_1255
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• 2009

The composites were fabricated by adding 30, 35, 40, 45[vol.%] Zirconium Diboride(hereafter, $ZrB_2$) powders as a second phase to Silicon Carbide(hereafter, SiC) matrix. The physical, mechanical and electrical properties of electroconductive SiC ceramic composites by Spark Plasma Sintering(hereafter, SPS) were examined. Reactions between $\beta$-SiC and $ZrB_2$ were not observed in the XRD analysis. The relative density of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites are 88.64[%], 76.80[%], 79.09[%] and 88.12[%], respectively. The XRD phase analysis of the electroconductive SiC ceramic composites reveals high of SiC and $ZrB_2$ and low of $ZrO_2$ phase. The electrical resistivity of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ composites are $6.74{\times}10^{-4}$, $4.56{\times}10^{-3}$, $1.92{\times}10^{-3}$ and $4.95{\times}10^{-3}[{\Omega}{\cdot}cm]$ at room temperature, respectively. The electrical resistivity of SiC+30[vol.%]$ZrB_2$, SiC+35[vol.%]$ZrB_2$, SiC+40[vol.%]$ZrB_2$ and SiC+45[vol.%]$ZrB_2$ are Positive Temperature Coefficient Resistance(hereafter, PTCR) in temperature ranges from 25[$^{\circ}C$] to 500[$^{\circ}C$]. It is convinced that SiC+40[vol.%]$ZrB_2$ composite by SPS can be applied for heater or electrode.

• Electrical & Electronic Materials
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• v.16 no.9
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• pp.64.2-65
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• 2003

A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{＋}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{＋}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.