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가습된 $N_2$/H$_2$혼합가스 분위기에서의 Kovar 산화 거동
김병수,김민호,김상우,최덕균,손용배 한국마이크로전자및패키징학회 2001 마이크로전자 및 패키징학회지 Vol.8 No.2
In order to form a uniform oxidation layer of spinel phase on Kovar which helps the strong bonding in Kovar-to-glass sealing, the humidified $N_2/H_2$ was used as an oxidation atmosphere. The oxidation of Kovar was controlled by diffusion mechanism and the activation energy was 31.61 kacl/mol at 500~$800^{\circ}C$. After oxidation at $600^{\circ}C$, the external oxidation layer was below 0.5 $\mu \textrm{m}$ thick. According to TEM analysis, oxidized Kovar was spinel its lattice parameter of 7.9 $\AA$. Oxidation of under $600^{\circ}C$ and in a humidified $N_2/H_2$ atmosphere, Kovar was found to be appropriate for the Kovar-to-glass sealing. 저열팽창성 금속인 Kovar표면을 유리와 접합하기에 적합한 spinel을 주상으로 하는 균일한 산화막을 형성할 수 있도록 $N_2/H_2$에 $H_2O$가 첨가된 분위기에서의 산화 거동에 대하여 조사하였다. Kovar 산화는 확산에 의해 지배되는 공정이며, 이때 산화 활성화 에너지는 31.61 kacl/mol 이었다. $600^{\circ}C$에서 열처리한 결과 spinel을 주상으로 하는 0.5 $mu extrm{m}$ 이하의 연속적이고 균일한 외부 산화막을 얻을 수 있었다. TEM 분석 결과 격자 상수가 7.9 $\AA$인 spinel 임을 확인할 수 있었다. 그러므로, 가습된 $N_2/H_2$분위기에서 산화한 Kovar는 유리와 접합에 적용 가능할 것으로 판단된다.
가습된 질소 분위기에서의 Kovar(Fe-29Ni-17Co)산화
김병수,김민호,김상우,최덕균,손용배 한국세라믹학회 1999 한국세라믹학회지 Vol.36 No.11
In order to form a uniform oxidation layer and spinel crystalline phase that was supposed to help strong bonding in Kovar(Fe-29Ni-17Co)to-glass sealing the humidified nitrogen (2.3%H2O/N2) was used as an oxidation atmosphere. Kovar oxidation was diffusion-contolled and the activation energy was 2.51 kcal/mol at 600-900$^{\circ}C$ After oxidation at 600$^{\circ}C$ the oxidation layer was under 1$\mu\textrm{m}$ thickness and crystalline phase was spinel which was found to be suitable for the Kovar-to-glass sealing.
적층형 셀과 아연도금층을 이용한 고온고압 합성다이아몬드의 압력변화에 따른 물성 연구
신운,송오성,Shen, Yun,Song, Oh-Sung 한국세라믹학회 2012 한국세라믹학회지 Vol.49 No.2
Fine diamond powders are synthesized with a 420 ${\phi}$ cubic press and stack-cell composed of Kovar ($Fe_{54}Ni_{29}Co_{17}$) (or Kovar+7 ${\mu}m$-thick Zn electroplated) alloy and graphite disks. The high pressure high temperature (HPHT) process condition was executed at $1500^{\circ}C$ for 280 seconds by varying the nominal pressure of 5.7~10.6 GPa. The density of formation, size, shape, and phase of diamonds are determined by optical microscopy, field emission scanning electron microscopy, thermal gravimetric analysis-differential thermal ammnlysis (TGA-DTA), X-ray diffraction (XRD), and micro-Raman spectroscopy. Through the microscopy analyses, we found that 1.5 ${\mu}m$ super-fine tetrahedral diamonds were synthesized for Zn coated Kovar cell with whole range of pressure while ~3 ${\mu}m$ super-fine diamond for conventional Kovar cell with < 10.6 GPa. Based on $750^{\circ}C$ exothermic reaction of diamonds in TGA-DTA, and characteristic peaks of the diamonds in XRD and micro-Raman analysis, we could confirm that the diamonds were successfully formed with the whole pressure range in this research. Finally, we propose a new process for super-fine diamonds by lowering the pressure condition and employing Zn electroplated Kovar disks.
저열팽창성 Fe-29Ni-17Co 코바 합금의 고온균열 발생과 고온연성에 미치는 S 및 Mn의 영향
이기안,박종혁,조봉현,남궁정,김문철 대한금속재료학회 2003 대한금속·재료학회지 Vol.41 No.12
The effect of S & Mn on the hot ductility of Fe-29Ni-17Co Kovar alloy and the mechanism of high temperature cracking occurrence were investigated. It has been found that the brittle intergranular fracture at high temperature cracking is closely associated with the sulfide along grain boundary. Experimental results showed, especially when the S content was high and the Mn content was free, that small cavities could be nucleated easily on FeS particles along grain boundary and propagated fast at high temperature. The hot ductility of Kovar alloy was drastically increased with the addition of Mn and it was also increased with decreasing S content. SEM and FE-SEM analyses showed that the Mn addition in this alloy could cause ductile intergranular fracture appearance below 1150℃ by the precipitation of MnS. It was proposed from the results that the addition of Mn and optimum S content (below 30 ppm) in Kovar alloy was necessary in order to reduce the hot cracking susceptibility.
Fe-Ni-Co 저열팽창성 합금의 고온 변형 특성 및 열간가공에 따른 열팽창 거동 연구
이기안,박종혁,조봉현,남궁정,김문철 대한금속재료학회 2003 대한금속·재료학회지 Vol.41 No.9
The high temperature deformation behavior and the effect of hot compression on the thermal expansion behavior of Fe-29Ni-17Co low thermal expansion Kovar alloy were investigated in the compressive temperature range of 900~1300℃ at the strain rate range of 25~0.01 sec.^(-1). The temperature (T) and strain rate (ε˙) dependence of the flow stress (σ_(0.7)) could be well described by hyperbolic sine law as ε˙= A [sinh(0.0084 σ)^(5.2018)] exp(-330.41/RT). Surface hot cracking and significant voids around grain boundary could be found at low temperature below 1000℃ and low strain rate (0.01 sec.^(-1)). Thermal expansion coefficient α_(30~400) generally increased with increasing compressive temperature. Moreover, α_(30~400) remarkably increased as strain rate decreased at high temperature above 1100℃. However the thermal expansion coefficient α_(30~400) of low compressive temperatures (900℃ and 1000℃) anomalously increased especially at high strain rates. Experimental results indicated that not only α phase appearance but also grain size had definite influence on the thermal expansion behavior with hot deformation. The correlation between microstructure and thermal expansion behavior of Kovar alloy were also discussed.