• 한국세라믹학회지
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• 제36권2호
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• pp.178-185
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• 1999

Si3N4 겔캐스팅공정 제어를 위하여, 슬립 조성의 영향이 슬립의 점성특성과 성형체의 기계적 특성 및 소결체의 밀도에 미치는 영향에 대하여 조사하였다. 아크릴아마이드 모노머, 고분자전해질, 그리고 질화규소의 혼합물을 어트리터에 예비혼합한 후 볼밀링하여 슬립을 제조하였다. 개시제가 혼합된 슬립을 진공탈포하고 몰드에 주입하고 중합을 진행하였으며, 겔화된 슬립을 건조하여 성형체를 얻었다. 슬립의 특성과 성형체의 기계적 특성을 평가하기 위해, 슬립의 점도 측정과 직경방향 압축시험을 행하였다. 그 결과, near net shaping을 위한 낮은 점도를 갖는 46 vol%의 고농도 질화규소 슬립의 제조가 가능하였다. 성형체가 기계적 특성은 주로 모노머의 농도에 비례하여 증가하였다. 또한, 겔캐스트 성형체의 인장강도가 약 3MPa이 넘으면 기계적 가공이 가능하였으며, 겔캐스팅 성형체를 176$0^{\circ}C$, 3시간 상압소결하여 약 98.5%의 상대밀도를 얻을 수 있었다.

• 한국분말재료학회지
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• 제22권4호
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• pp.283-288
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• 2015

Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-TiC composite powders which are fabricated by high-energy ball-milling. A powder mixture of Fe and TiC is prepared in a planetary ball mill at a rotation speed of 500 rpm for 1h. Pressureless sintering is performed at 1100, 1200 and $1300^{\circ}C$ for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of $1050^{\circ}C$, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of $50^{\circ}C$, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts show incomplete densification with a relative denstiy of 86.1% after sintering at $1300^{\circ}C$ for 3h. Spark-plasma sintering at $1050^{\circ}C$ for 10 min exhibits nearly complete densification of 98.6% relative density under the sintering pressure of 50 MPa.

• 한국세라믹학회지
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• 제48권5호
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• pp.368-372
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• 2011

Aluminum nitride (AlN) has excellent thermal conductivity, whereas it has some disadvantage such as low sinterability. In this study, the effects of sintering additive content and sintering condition on thermal conductivity of pressureless sintered AlN ceramics were examined on the variables of 1~3 wt% sintering additive ($Y_2O_3$) content at $1900^{\circ}C$ in $N_2$ atmosphere with holding time of 2~10 h. All AlN specimens showed higher thermal conductivity as the $Y_2O_3$ content and holding time increase. The formation of secondary phases (yttrium aluminates) by reaction of $Y_2O_3$ and $Al_2O_3$ from AlN surface promoted the thermal conductivity of AlN specimens, because the secondary phases could reduce the oxygen contents in AlN lattice. Also, thermal conductivity was increased by long sintering time because of the uniform distribution and the elimination of the secondary phases at the grain boundary by the evaporation effect during long holding time. A carbothermal reduction reaction was also affected on the thermal conductivity. The thermal conductivity of AlN specimens sintered at $1900^{\circ}C$ for 10 h showed 130~200W/mK according to the content of sintering additive.

• 한국분말재료학회지
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• 제26권5호
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• pp.395-404
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• 2019

Aluminum nitride (AlN) has excellent electrical insulation property, high thermal conductivity, and a low thermal expansion coefficient; therefore, it is widely used as a heat sink, heat-conductive filler, and heat dissipation substrate. However, it is well known that the AlN-based materials have disadvantages such as low sinterability and poor mechanical properties. In this study, the effects of addition of various amounts (1-6 wt.%) of sintering additives $Y_2O_3$ and $Sm_2O_3$ on the thermal and mechanical properties of AlN samples pressureless sintered at $1850^{\circ}C$ in an $N_2$ atmosphere for a holding time of 2 h are examined. All AlN samples exhibit relative densities of more than 97%. It showed that the higher thermal conductivity as the $Y_2O_3$ content increased than the $Sm_2O_3$ additive, whereas all AlN samples exhibited higher mechanical properties as $Sm_2O_3$ content increased. The formation of secondary phases by reaction of $Y_2O_3$, $Sm_2O_3$ with oxygen from AlN lattice influenced the thermal and mechanical properties of AlN samples due to the reaction of the oxygen contents in AlN lattice.

• 한국재료학회지
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• 제9권8호
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• pp.817-824
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• 1999

$Al_2$$O_3$-SiC 화합물 분말이 $SiO_2$, A1 그리고 C 분말들을 원료분말로 하여 SHS(self-propagating High-temperature Synthesis)법에 의해 제조되었다. 원료 분말에서의 몰비, 성형압력, 반응물의 초기온도의 영향이 생성물과 연소과정에 대해 연구되었다. $SiO_2$/A1/C계의 자전연소합성은 낮은 연소온도 때문에 $400^{\circ}C$ 이상으로 예열되어야 한다. 연소반응의 결과로서 최종생성물의 순도는 반응물의 순도보다 높았다. 이 계에서 $SiO_2$:Al:C의 적당한 몰비는 3.0:4.0:6.0이었고, free carbon은 30min 동안 $650^{\circ}C$에서 배소함으로써 제거되었다. 본 연구에서 상압소결은 $1700^{\circ}C$에서 powder bed를 사용한 표본의 분해를 제어하고 치밀한 소결체를 얻는데 매우 효과적이었다. hot-pressing으로 생성된 소결체는 이론비교밀도의 약 98%이었다.

• 한국세라믹학회지
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• 제33권8호
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• pp.921-927
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• 1996

The liquid-phase concentration from the interior to the surface region and its influence on the microstructural changes were investigated in pressureless sintered $\beta$-SiC Surface reaction-layer was formed by reaction of packing powder and volatile components on the surface during sintering which was induced the concentration of liquid-phase in the surface regions. The microstructural changes between the surface region and the interior were appeared in sintered specimen which was resulted from the difference of liquid-phase content during sintering. Microstructural changes were observd with the depth of about 250${\mu}{\textrm}{m}$ from he surface. The grain size and aspect ratio of SiC in the interior are larger than those in the surface region and the rate of transforma-tion of $\beta$-to $\alpha$-SiC during sintering is higher in the interior than that in the surface region.

• 한국세라믹학회지
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• 제31권5호
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• pp.552-560
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• 1994

A composite of TiB2-Al2O3 system was successfully prepared from a mixture of TiO2, B2O3, and Al by self-propagating high temperature synthesis (SHS) with a novel characteristic, utilizing the internal oxidation heat of aluminium metal of the mixture, instead of by a conventional technique, externally heating a mixture of Ti, B and Al2O3. From a mixture with B/Ti molar ratio of =2.0, pure two phases of TiB2 and $\alpha$-Al2O3 with good crystallinity and small, uniform sizes were formed. However, when the B/Ti molar ratio of the mixture goes to a value less than 2.0, in addition to the above main minerals, a small smounts of metastable phases such as TiB and Ti3B4 were formed. It was found that about 60%, the optimum green density of compacts gave their highest reaction rate and temperature during SHS process. TiB2-Al2O3 system composite with B/Ti molar ratio of =2.0 could be pressurelessly sintered even at 190$0^{\circ}C$ under Ar gas flows without any addition of sintering aids, showing their good properties such as 91.2% in relative density, 2750 kgf/$\textrm{mm}^2$ in Vickers hardness and 2620 kgf/$\textrm{cm}^2$ in flexural strength.

• 한국세라믹학회지
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• 제36권1호
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• pp.15-20
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• 1999

상압소결 질화규소에 대한 고온정피로 거동을 K-t(stress intensity/life test)법에 의해 조사하였다. 정피로 크랙성장속도는 온도의 증가와 함께 증가한다. 온도의 증가에 따라 크랙성장속도가 증가하는 이유는 온도 증가에 따라 파괴인성치가 감소하기 때문으로 판명되었다. 즉 정피로 크랙성장속도 da/dt를 da/dt=AK1m로 나타내면, 이 식의 정수 A는 파괴인성치의 파괴인성치의 함수이도, 지수 m은 온도나 파괴인성치에 관계없이 일정한 상수이다. 그러나 글래스상의 연화가 일어나는 고온의 경우 크랙성장속도는 이상의 관계로부터 벗어남을 발견하고, 그 이유에 대하여 고찰하였다.

• 한국세라믹학회지
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• 제36권5호
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• pp.547-554
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• 1999

The self-reinforced Si3N4 ceramics were prepared by pressureless-sintering using ${\beta}$-Si3N4 whiskers as a seed. Effects of ${\beta}$-Si3N4 whiskers on microstructure and mechanical properties and the ${\alpha}$ to ${\beta}$ phase transition of Si3N4 were investigated. The self-reinforced Si3N4 ceramics were densified(relative density$\geq$98%) by pressureless-sintering (1800$^{\circ}C$ 2h) using 8mol% Y2O3 and 6mol% Al2O3 as sintering aids and 5 vol% ${\beta}$-Si3N4 whiskers within self-reinforced Si3N4 ceramic seemed to hinder the densification owing to their acicular shapes but accelerated the ${\alpha}$ to ${\beta}$ phase transition because they acted as pre-existing nuclei. It was found that the more ${\beta}$-Si3N4 nucei the faster ${\alpha}$ to ${\beta}$ phase transition.

• 한국세라믹학회지
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• 제34권7호
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• pp.781-789
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• 1997

Pressure sintered SiC specimens were joined using MgO-Al2O3-SiO2 (MAS) glass which has a thermal expansion coefficient similar to that of SiC. MAS melt showed excellent behavior of wetting on the SiC substrate over 148$0^{\circ}C$, and the wettability was much influenced by the joining atmosphere. The joining was conducted at 150$0^{\circ}C$ for 30 min in Ar atmosphere. The flexural strength of the joined specimen shows 342~380 MPa up to 80$0^{\circ}C$, which is almost the same as that of as-recieved SiC specimen. However, the flexural strength of the joined specimen decreased to about 80 MPa at 90$0^{\circ}C$ due to softening of the glass melt. The analyses od XRD and WDS show that the reaction between the SiC specimen and the MAS melt produces the oxycarbide glass, which had a high strength and a good stability at high temperatures.