• 한국분말재료학회지
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• 제19권1호
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• pp.25-31
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• 2012

In this study, a high energy ball milling process was employed in order to improve the densification of direct nitrided AlN powder. The densification behavior and the sintered microstructure of the milled AlN powder were investigated. Mixture of AlN powder doped with 5 wt.% $Y_2O_3$ as a sintering additive was pulverized and dispersed up to 50 min in a bead mill with very small $ZrO_2$ beads. Ultrafine AlN powder with a particle size of 600 nm and a specific surface area of 9.54 $m^2/g$ was prepared after milling for 50 min. The milled powders were pressureless-sintered at $1700^{\circ}C-1800^{\circ}C$ for 4 h under $N_2$ atmosphere. This powder showed excellent sinterability leading to full densification after sintering at $1700^{\circ}C$ for 4 h. However, the sintered microstructure revealed that the fraction of yitttium aluminate increased with milling time and sintering temperature and the newly-secondary phase of ZrN was observed due to the reaction of AlN with the $ZrO_2$ impurity.

• 한국산학기술학회논문지
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• 제12권12호
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• pp.5438-5442
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• 2011

자동차용 경량소결부품으로 사용하기 위하여 2712 Al 합금 및 2712에 세라믹스를 각각 10, 20, 33% 첨가한 소결체의 기계적 특성에 대하여 조사하였다. 그 결과, (1)모든 소결체에서 4~7%의 기공이 잔류하는 것을 발견하였다. (2)시효처리한 2712 소결체 및 10, 20, 33% 세라믹스 함유 소결체의 인장강도 값은, 12분 소결에서는 각각 165, 260, 256, 166 N/$mm^2$, 30분 소결에서는 각각 186, 229, 219, 202 N/$mm^2$로 나타나, 세라믹스를 10% 첨가하여 12분 소결한 경우가 가장 우수한 인장강도 값을 나타내었다. 또한, 소결체의 최대 연신율값 3.6%는 세라믹스를 10% 첨가하여 30분 소결 후 시효처리한 소결체에서 나타났다. (3)시효처리 후의 소결체 표면의 최대 겉보기 경도값 ($H_RF$) 97은 세라믹스를 10% 첨가하고 30분 소결한 경우에 나타났다. (4)가장 낮은 내마모량 값 $174{\times}10^{-3}mm^3$은 10% 세라믹스를 첨가하여 시효처리한 소결체에서 나타났다. 이러한 결과들로부터 세라믹스를 10% 첨가한 2712 소결체가 Al 엔진부품 제조에 가장 적합한 것으로 판단되었다.

• 한국세라믹학회지
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• 제48권5호
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• pp.418-425
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• 2011

In this study, a high energy ball milling process was introduced in order to improve the densification of direct nitrided AlN powder. The sintering behavior and thermal conductivity of the AlN milled powder was investigated. The mixture of AlN powder and 5 wt% $Y_2O_3$ as a sintering additive was pulverized and dispersed by a bead mill with very small $ZrO_2$ bead media. The milled powders were sintered at $1700^{\circ}C-1800^{\circ}C$ for 4 h under $N_2$ atmosphere. The results showed that the sintered density was enhanced with increasing milling time due to the particle refinement as well as the increase in oxygen contents. Appropriate milling time was effective for the improvement of thermal conductivity, but the extensive millied powder formed more fractions of secondary phase during sintering, resulted in the decrease in thermal conductivity. The AlN powder milled for 10min after sintering at $1800^{\circ}C$ revealed the highest thermal conductivity, of 164W/$m{\cdot}K$ in tne densified AlN sintered at $1800^{\circ}C$.

• 한국세라믹학회지
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• 제28권3호
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• pp.189-196
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• 1991

Si(OC2H5)4, commercial AlN and Y2O3 powder were used as the precusor of Si3N4, AlN, Y2O3, respectively. After Si3N4 powder was synthesized by carbothermal reduction and nitridation at 135$0^{\circ}C$ for 13h in N2 atmosphere, characteristics of synthesized powder and the ceramics sintered at 178$0^{\circ}C$ for 1h under 30MPa were investigated. In order to evaluate the reliability of sintered body, Weibull modulus was investigated. Premixing of carbon black as a reduction agent had no effect on Si(OH)4 formation, and Si3N4 powder synthesized from Si(OC2H5)4 was $\alpha$-Si3N4 single phase. Mechanical properties of sintered body were measured as follows : flexural strength ; 750MPa, fracture toughness ; 3.71Mn/3/2, hardness : 17.4GPa, thermal shock resistence temperature ; $600^{\circ}C$. Flexural strength at room temperature was 750MPa and was retained up to 110$0^{\circ}C$. The Weibull modulus of sintered body was 10.7.

• 한국세라믹학회지
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• 제33권2호
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• pp.169-176
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• 1996

The specimens which were prepared from $\alpha$-Si3N4 with additions of YAG(3Y2O3.5Al2O3)-10 wt% and various AlN contents were sintered in N2 atmosphere at 1$700^{\circ}C$ The effect of $\alpha$,$\beta$-solid solution contents and sintering time on mechanical properties were investigated. As the content of $\beta$-solid solution and sintering time increased the hardness is reduced but the hardness of specimen sintered over 10 hours is constant irrespective of sintering time. While the fracture toughness increased with increasing of $\beta$-solid solution and sintering time. The fracture toughness of specimen with 80% $\beta$-solid solution content increased from 3.89 to 6.66 MPam1/2 with sintering sintering up to 20 hours/ But the amount of increased fracture toughness of specimen with below 20% $\beta$-solid solution content is not significant.

• 한국분말재료학회지
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• 제18권4호
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• pp.365-371
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• 2011

In this study, gradient porous Al-Cu sintered body was fabricated by powder metallurgy processing. Al-Cu powder mixtures were prepared by low energy ball milling with various milling time. After ball milling for 3h, the shape of powder mixtures changed to spherical type with size of 100~500 ${\mu}m$. Subsequently, Al-Cu powder mixtures were classified (under 150, 150~300 and over 300 ${\mu}m$) and compacted (20, 50 and 100 MPa). Then, they were sintered at $600^{\circ}C$ for various holding time (10, 30, 60 and 120 min) in $N_2$ atmosphere. The sintered bodies had 32~45% of porosity. As a result, the optimum holding time was determined to be 60 min at $600^{\circ}C$ and sintered bodies with various porosity were obtained by controlling the compacting pressure.

• 분석과학
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• 제6권2호
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• pp.207-215
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• 1993

소결첨가제($3Al_2O_3{\cdot}5Y_2O_3$, YAG)를 질화규소에 공침방법으로 첨가하여, 통상적인 기계적 혼합 방법으로 준비된 혼합분말에 대한 혼합균일성과 소결 및 기계적 특성을 조사, 비교하였다. 준비된 혼합분말들을 SIMS를 사용하여 분말 표면과 내부의 조성을 비교분석한 결과, 공침법을 사용할 경우 소결첨가제가 $Si_3N_4$ 표면에 피복된 상태로 존재하고 있음을 나타내어 기계적 혼합에 비해 우수한 균일혼합효과를 얻을 수 있음을 확인하였다. 공침법에 의한 균일혼합효과는 $Si_3N_4$ 분말소결체의 소결밀도 및 미세구조의 개선을 수반하여 기계적 강도의 향상을 이룰 수 있음을 확인하였다.

• 한국세라믹학회지
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• 제53권6호
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• pp.635-640
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• 2016

Electrical behavior of AlN ceramics sintered with $Y_2O_3$ as a sintering aid has been investigated with respect to additional $TiO_2$ dopant. From the impedance spectroscopy, it was found that the grain and grain boundary conductivities have greatly decreased with addition of $TiO_2$ dopant. The $TiO_2$ dopant also increased the activation energy of the grain conductivity by about 0.37 eV; this increase was attributed to the formation of an associate between Al vacancies and Ti ions at the Al sites. Similarly, the electronic conductivity was reduced by $TiO_2$ addition. However, $TiO_2$ solubility in AlN grains was below the detection limit of typical EDX analysis. Grain boundary was clean, without liquid films, but did show yttrium segregation. The transference number of ions was close to 1, showing that AlN is a predominantly ionic conductor. Based on the observed results, the implications of using AlN applications as insulators have been discussed.

• 한국세라믹학회지
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• 제36권2호
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• pp.193-202
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• 1999

Al 분말과 AlN 분말에 SiC 휘스커와 소결조제를 첨가하여 습식혼합한 후 성형체를 제조하고 600~140$0^{\circ}C$의 온도에서 5시간 동안 질화반응을 진행시켰다. 반응소결체의 꺾임강도를 측정한 결과 질화율이 높아질수록, 그리고 SiC 휘스커의 첨가량이 많아질수록 증진되는 것을 확인할 수 있었다. Al과 AlN이 50:50으로 혼합된 시편을 140$0^{\circ}C$에서 5시간 동안 질화반응을 시킨 결과 97% 이상의 질화율과 2%미만의 수축율을 나타내었고, 상대밀도값은 78%이었다. 그리고 반응소결체의 최대 꺾임강도는 250 MPa이었다. 완전히 질화반응을 시켜 미반응 Al이 잔존하지 않는 시편들을 1$700^{\circ}C$, 180$0^{\circ}C$, 190$0^{\circ}C$의 온도에서 2시간 동안 재소결한 결과 수축은 6% 미만이었으며, 최고 86%의 상대밀도를 나타내었다. 180$0^{\circ}C$이상의 온도에서 2시간 동안 재소결한 결과 수축은 6%미만이었으며, 최고 86%의 상대밀도를 나타내었다. 180$0^{\circ}C$이상의 온도에서 재소결한 시편들의 경우 AlN과 SiC 휘스커가 고용체를 형성하여 SiC 휘스커 첨가에 의한 기계적 물성의 증진 효과는 거의 나타나지 않았다. 그리고 재소결한 시편의 최대 꺾임강도는 295 MPa이었다.

• 한국세라믹학회지
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• 제28권6호
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• pp.457-464
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• 1991

Aluminum nitride (AlN) has excellent properties such as high thermal conductivity and electrical resistivity, whereas it has some disadvantages such as low sinterability and tendency to be hydrolyzed by moisture at room temperature. In the present work, the relative density, modulus of rupture and microhardness were examined for pressure-less-sintered AlN (synthetic and commercial) bodies which were prepared under the conditions of various sintering temperatures, holding times and additions of CaCO3 which showed the best effect on sinterability among the various sintering aids. As a result, the AlN bodies with 1.0 wt% CaCO3 (0.56wt% CaO) which were sintered at 1800$^{\circ}C$ for 20 min showed good densification. In this case, the relative densities were 95.9% and 95.2%, and microhardnesses were 10.3 GPa and 9.8 GPa for synthetic and commercial AlN respectively. And as the holding time at 1800$^{\circ}C$ was increased from 10 min to 60 min, the relative density was increased from 91.9% to 96.5%. It was considered that impurities of metals and oxygen promoted the densification of AlN at low temperature (1600$^{\circ}C$).