The semiconductor and display industries require the development of plasma resistant materials for use in high density plasma etching process equipment. Yttria (Y2O3) is a ceramic material mainly used to ensure good plasma resistance properties, which requires a dense microstructure. In commercial production, a sintering process is applied to reduce the sintering temperature of Y2O3. In this study, the effect of the addition of glass frit to the sintered specimen was examined when manufacturing yttria sintered specimens for semiconductor process equipment parts. The Y2O3 specimen was shaped into a Ø50 mm size and then sintered at 1,600 °C for 1~8 h. The characteristics, X-ray diffraction pattern, densities, contraction rate of the specimen, and swelling of the surface of the Y2O3 specimens were investigated as a function of the sintering time and glass frit addition. The Y2O3 specimen exhibited a density of over 4.9 g/cm3 as the sintering time increased, and the swelling phenomenon characteristics were improved by glass frit, by controlling particle size.
In this study, the effect of the content of MgO-CaO-Al2O3-SiO2 (MCAS) glass additives on the properties of AlN ceramics is investigated. Dilatometric analysis and isothermal sintering for AlN compacts with MCAS contents varying between 5 and 20 wt% are carried out at temperatures ranging up to 1600℃. The results showed that the shrinkage of the AlN specimens increases with increasing MCAS content, and that full densification can be obtained irrespective of the MCAS content. Moreover, properties of the AlN-MCAS specimens such as microhardness, thermal conductivity, dielectric constant, and dielectric loss are analyzed. Microhardness and thermal conductivity decrease with increasing MCAS content. An acceptable candidate for AlN application is obtained: an AlN-MCAS composite with a thermal conductivity over 70 W/m·K and a dielectric loss tangent (tan δ) below 0.6 × 10−3, with up to 10 wt% MCAS content.
In this study, MgO–CaO–Al2O3–SiO2 (MCAS) nanocomposite glass powder having a mean particle size of 50 nm and a specific surface area of 40 m2/g is used as a sintering additive for AlN ceramics. Densification behaviors and thermal properties of AlN with 5 wt% MCAS nano-glass additive are investigated. Dilatometric analysis and isothermal sintering of AlN-5wt% MCAS compact demonstrates that the shrinkage of the AlN specimen increases significantly above 1,300oC via liquid phase sintering of MCAS additive, and complete densification could be achieved after sintering at 1,600oC, which is a reduction in sintering temperature by 200oC compared to conventional AlN-Y2O3 systems. The MCAS glass phase is satisfactorily distributed between AlN particles after sintering at 1,600oC, existing as an amorphous secondary phase. The AlN specimen attained a thermal conductivity of 82.6 W/m·K at 1,600oC.
Glass-ceramics were fabricated by heat-treatment of glass obtained by melting a coal bottom ash with Li2O addition. The main crystal grown in the glass-ceramics, containing 10 wt% Li2O, was β-spodumene solid solution, while in Li2O 20 wt% specimen was mullite, identified using XRD. The activation energy and Avrami constant for crystallization were calculated and showed that bulk crystallization behavior will be predominant, and this expectation agreed with the microstructural observations. The crystal phase grown in Li2O 10 wt% glass-ceramics had a dendrite-like shaped whereas the shape was flake-like in the 20 wt% case. The thermal expansion coefficient of the Li2O 10 wt% glass-ceramics was lower than that of the glass having the same composition, owing to the formation of a β-spodumene phase. For example, the thermal expansion coefficient of Li2O 10 wt% glass-ceramics was 20×10-7, which is enough for application in various heat-resistance fields. But above 20 wt% Li2O, the thermal coefficient expansion of glass-ceramics, on the contrary, was higher than that of the same composition glass, due to formation of mullite.
The effects of thermal properties on the crystallization behavior of CaMgSi2O6 glass-ceramics were investigated as a function of sintering temperature from 800˚C to 900˚C. The crystallization behavior of the specimens depended on the sintering temperature, which could be evaluated from the differential thermal analysis, X-ray diffraction and Fourier transform infrared spectroscopy. With increasing sintering temperature, the thermal conductivity of the sintered specimens increased, while the coefficient of thermal expansion (CTE) of the sintered specimens decreased. These results could be attributed to the increase of crystallization, confirmed from the estimation by density measurements. Also, the thermal diffusivity and specific heat capacity of the sintered specimens were discussed with relation to the sintering temperature. Typically, a thermal conductivity of 3.084 W/m˚C, CTE of 8.049 ppm/˚C, thermal diffusivity of 1.389 mm2/s and specific heat capacity of 0.752 J/g˚C were obtained for CaMgSi2O6 specimens sintered at 900˚C for 5 h.
Glass ceramics were made from coal bottom ash by adding CaO and Li2O as glass modifiers and TiO2 as a nucleating agent in a process of melting and quenching followed by a thermal treatment. The surface of the glass ceramics has 1.6 times more Li2O compared to the inner matrix. When TiO2 was not added or when only 2 wt% was added, the surface parts of the glass ceramics were crystalline with a thickness close to 130μm. In addition, the matrixes showed only the glass phase and not the crystalline phase. However, doping of TiO2 from 4 wt% to 10 wt% began to create small crystalline phases in the matrix with an increase in the quantity of the crystalline. The matrix microstructure of glass ceramics containing TiO2 in excess of 8 wt% was a mixture of dark-gray crystalline and white crystalline parts. These two parts had no considerable difference in terms of composition. It was thought that the crystallization mechanism affects the crystal growth, direction and shape and rather than the existence of two types of crystals.
The shrinkage variation of Low Temperature Cofired Ceramics(LTCC) limits the size of the substrates that impose limitations on embedded passive components. This paper focuses on the method of minimizing or controlling planar shrinkage and reducing distortion during firing. The laminated sheets of alumina and glass were sintered at varying temperature, and depending on the amount of the glass ceramics. When the sintered of multi-layer structure with , the glass infiltrated entirely into layer at the temperature of about or higher.
고온 안정성의 유리계로 알려진 회토류 알루미나 규산염계중, Nd2O3-Al2O3-SiO2(NdAS)계 유리의 응용범위를 찾고자 결정화유리를 제조하여 그 물성의 특성을 평가하였다. NdAS에 결정화제로 TiO2를 첨가하여 내부결정화를 유도하여 생성된 결정화유리에 대하여 결정상과 잔류유리의 물리적, 열적, 기계적 물성을 측정하였다. NdAS-TiO2유리계는 열처리와 조성 조건에 따라 생성된 표면 및 내부결정상은 같은 결정상을 갖는 것으로 X선회절의 결과로 확인되었으나, 알려 있지 않은 결정상으로 내부결정의 경우, 원자구성비는 Nd4.6Si7.2Al4.0Ti2.4O32이었다. 결정화유리의 선팽창계수는 5.4~6.2×10-6/˚C 정도로 경정성장이 일어날수록 증가되었다. 결정화유리중의 결정상의 경도와 탄성계수는각 각 12GPa, 220Gpa으로 나타난 것을 고려한다면 내부결정화에 의한 결정화유리의 물성은 고온 구조용 재료로 활용도가 넓을 것으로 본다.
본 연구는 이온교환에 의한 Li2O-AI2O3 계 결정화유리의 강화에 관한 연구이다. 모유리의 이온교환 전후의 강도를 비교하였으며, 결정화유리의 결정화전후에 이온교환에 따르는 강도를 상호 비교하였다. 그 결과 모유리의 Na+이온교환에 따른 최대 강도값은 450˚C-3hr의 열처리 조건하에서 최고 6배(60Kg/mm2)의 강도값을 나타내었으며, 결정화후 이온교환에 따른 강도증가는 450˚C-1hr의 열처리 조건하에서 최고 10배의 강도증대효과를 보였다. 한편 과도한 이온교환 열처리조건하에서는 응력이완현상을 나타냄을 알 수 있었다.
Li2O-Al2O3-SiO3계 결정화유리의 저온합성을 위하여 출방원료로서 각 해당 금속 알콕시드를 사용하였다. 알코올을 용매로 충분히 첨가하고, drying control chemical additive로 dimethy1 formamide를 적당량 첨가한 혼합용용액을 과잉의 물로 충분히 가수분해시킨 습윤겔을 저온으로 건고하여 균열이 없는 건조된 monolith겔을 합성하였다. 건조겔로부터 750-950˚C로 10시간 이상 소결하여 저열팽창성을 나타내는 β-eucrypytite(β-quartz 고용체), Li2O· Al2O3· 3SiO2및 β-spodumene등의결정상을 석출시켰다.