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SHS 공정에 의해 제조된 Mo<sub>x</sub>W<sub>1-x</sub>Si<sub>2</sub> 발열체의 열화메커니즘
이동원,이상헌,김용남,이성철,구상모,오종민,Lee, Dong-Won,Lee, Sang-Hun,Kim, Yong-Nam,Lee, Sung-Chul,Koo, Sang-Mo,Oh, Jong-Min 한국전기전자재료학회 2017 전기전자재료학회논문지 Vol.30 No.10
The degradation mechanism of $Mo_xW_{1-x}Si_2$ ultrahigh-temperature heating elements fabricated by self-propagating high-temperature synthesiswas investigated. The $Mo_xW_{1-x}Si_2$ specimens (with and without post-annealing) were subjected to ADTs (accelerated degradation tests) at temperatures up to $1,700^{\circ}C$ at heating rates of 3, 4, 5, 7, and $14^{\circ}C/min$. The surface loads of all the specimen heaters were increased with the increase in the target temperature. For the $Mo_xW_{1-x}Si_2$ specimens without annealing, many pores and secondary-phase particles were observed in the microstructure; the surface load increased to $23.9W/cm^2$ at $1,700^{\circ}C$, while the bending strength drastically reduced to 242 MPa. In contrast, the $Mo_xW_{1-x}Si_2$ specimens after post-annealing retained $single-Mo_xW_{1-x}Si_2$ phases and showed superior durability after the ADT. Consequently, it is thought that the formation of microcracks and coarse secondary phases during the ADT are the main causes for the degraded performance of the $Mo_xW_{1-x}Si_2$ heating elements without post-annealing.
SHS 공정으로 제조된 Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si₂ 발열체의 가속수명시험과 고장분석
이동원(Dong-Won Lee),이상헌(Sang-Hun Lee),김용남(Yong-Nam Kim),이희수(Heesoo Lee),이성철(Sung-Chul Lee),구상모(Sang-Mo Koo),오종민(Jong-Min Oh) 한국전기전자학회 2017 전기전자학회논문지 Vol.21 No.3
고온자전합성과 후열처리 공정으로 MoxW1-xSi₂ 발열체를 제조하였다. MoxW1-xSi₂ 발열체의 신뢰성을 검증하기 위해 가속수명시험을 수행하였으며, 수명시간을 Minitab 프로그램으로 추정하였다. 또한, 가속수명시험 후의 MoxW1-xSi₂ 발열체의 고장분석을 전기적과 구조적 특성으로부터 수행하였다. 그 결과, MoxW1-xSi₂ 발열체의 지배적인 고장 유형은 발열체 내부의 크랙 형성과 SiO₂ 보호층의 박리임을 확인하였다. MoxW1-xSi₂ heaters were fabricated by self-propagating high-temperature synthesis (SHS) process and post sintering process. To validate the reliability of the MoxW1-xSi₂ heaters, the accelerated life test (ALT) was conducted, and then lifetime to MoxW1-xSi₂ heaters was estimated by using Minitab programs. Also, the failure analysis of MoxW1-xSi₂ heaters after ALT was performed through electrical and structural properties. As the results, it was confirmed that the dominant failure mode of MoxW1-xSi₂ heaters is the crack formation in heaters and the delamination of protective SiO₂ layers.
Cho, Myung-Yeon,Lee, Sung-Chul,Park, Chulhwan,Lee, Daeseok,Koo, Sang-Mo,Moon, Kyoung-Sook,Lee, Dong-Won,Oh, Jong-Min Elsevier 2019 INTERMETALLICS Vol.110 No.-
<P><B>Abstract</B></P> <P>High-performance tungsten molybdenum disilicide (Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB>) heating elements were prepared using a self-propagating high temperature synthesis process. The effect of post annealing on the degradation behavior of the alloy was experimentally investigated. Increasing the attrition milling time up to 20 min during powder preparation resulted in Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB> heaters with the highest density, which increased the fracture strength compared to samples with shorter attrition times. Such samples were annealed and evaluated as heating elements using accelerated degradation tests and failure analysis in order to compare their structural characteristics and flexural strength with as-fabricated samples. The annealed Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB> heater showed a relatively dense structure with few pores and no secondary phases, apart from a SiO<SUB>2</SUB> layer. This favorable structure prevented bubble formation, which can result in fracturing of the heater, as revealed by evaluation at high temperatures with various heating rates. The flexural strength of the annealed specimen was 2.5-times higher than that of the as-fabricated specimen, which was attributed to removal of secondary phases during annealing. Failure time and surface load analyses were used to investigate the fracture mechanism of the Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB> heaters in detail at 1790 °C by quantifying bubble formation and the presence of secondary phases.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Self-propagating high temperature synthesis of Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB> heaters demonstrated. </LI> <LI> Post-annealed Mo<SUB>x</SUB>W<SUB>1-x</SUB>Si<SUB>2</SUB> heaters were highly dense, with good flexural strength. </LI> <LI> Bubble formation (the main cause of fracture) suppressed at ultra-high temperature (above 1700 °C). </LI> <LI> Surface load, failure time, and bubble formation used to study fracture mechanisms. </LI> </UL> </P>