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1.
Powder compacts consisting of Al, Al2 O3 , and ZrO2 were heated by microwave radiation. Tracing the phase evolution during reaction bonding revealed the reaction mechanism. In the case of conventional heating, the compacts expanded slightly at temperatures of <700°C due to Al surface oxidation and expanded sharply at temperatures greater than 700°C as oxidation proceeded from the surface to the interior. Then, the compacts shrank at 1550°C due to sintering. For the case of microwave heating, the compacts expanded at temperatures of <550°C due to the formation of Al3 Zr. This Al3 Zr formation was caused by the preferential heating of ZrO2 relative to Al and Al2 O3 by microwave radiation. Then, Al3 Zr was oxidized to form Al2 O3 and ZrO2 at temperatures of >1000°C. Finally, the compacts shrank at 1550°C due to sintering, similarly to conventional sintering. 相似文献
2.
D.W. JOHNSON JR. E.M. RABINOVICH J.B. MacCHESNEY E.M. VOGEL 《Journal of the American Ceramic Society》1983,66(10):688-693
The sintering of dried colloidal SiO2 gels, whose preparation and properties are reported in Part I, is described. The effects of various sintering parameters were studied and the conditions for achievement of the best optical quality include the use of: a pretreatment of the SiO2 at ∼925°C, moderate heating rate (∼400°C/h), He+CI2 atmosphere, 1500° to 1600°C sintering temperature, and 1 to 4 h sintering time. Dynamic sintering kinetic studies (heating rate=400°C/h) show that this SiO2 sinters to nearly theoretical density by about 1380°C. However, optical transparency is achieved by removal of minor residual porosity at above 1500°C. Isothermal sintering data fit to a model assuming interconnecting cylinders of SiO2 predict the proper activation energy for the viscosity if initial stages of sintering are considered. Residual porosity in sintered glasses is related to large interstices in the unsintered gel. 相似文献
3.
Pressureless Sintering of Boron Carbide 总被引:4,自引:0,他引:4
B4 C powder compacts were sintered using a graphite dilatometer in flowing He under constant heating rates. Densification started at 1800°C. The rate of densification increased rapidly in the range 1870°–2010°C, which was attributed to direct B4 C–B4 C contact between particles permitted via volatilization of B2 O3 particle coatings. Limited particle coarsening, attributed to the presence or evolution of the oxide coatings, occurred in the range 1870°–1950°C. In the temperature range 2010°–2140°C, densification continued at a slower rate while particles simultaneously coarsened by evaporation–condensation of B4 C. Above 2140°C, rapid densification ensued, which was interpreted to be the result of the formation of a eutectic grain boundary liquid, or activated sintering facilitated by nonstoichiometric volatilization of B4 C, leaving carbon behind. Rapid heating through temperature ranges in which coarsening occurred fostered increased densities. Carbon doping (3 wt%) in the form of phenolic resin resulted in more dense sintered compacts. Carbon reacted with B2 O3 to form B4 C and CO gas, thereby extracting the B2 O3 coatings, permitting sintering to start at ∼1350°C. 相似文献
4.
The effect of heating rate (2 to 30°C/min) during sintering on the perovskite phase content, density, microstructure, and dielectric properties of 0.9PbMg1/3 Nb2/3 O3 –0.1PbTiO3 relaxor ferroelectric ceramics has been studied. Increasing the heating rate reduced the level of PbO evaporation and resulted in high perovskite content and dense ceramics. With slow heating rate (2–10°C/min), excess MgO segregated as isolated submicrometer particles in the perovskite grains; these precipitates were absent in ceramics sintered with a heating rate of 30°C/min. The maximum dielectric constant was optimized with a heating rate of 10°C/min. The temperature of maximum dielectric constant shifted downward as the heating rate was increased. 相似文献
5.
Satoru Fujitsu Makoto Ikegami Takashi Hayashi 《Journal of the American Ceramic Society》2000,83(8):2085-2087
Partially stabilized zirconia (PSZ) powders were fully densified by microwave heating using a domestic microwave oven. Pressed powder compacts of PSZ were sandwiched between two ZnO–MnO2 –Al2 O3 ceramic plates and put into the microwave oven. In the first step, PSZ green pellets were heated by self-heating of ZnO–MnO2 –Al2 O3 ceramics (1000°C). In the second step, the heated PSZ pellets absorbed microwave energy and self-heated up to a higher temperature (1250°C), leading to densification. The density of PSZ obtained by heating in the microwave oven for 16 min was 5.7 g/cm3 , which was approximately equal to the density of bodies sintered at 1300°C for 4 h or 1400°C for 16 min by the conventional method. The average grain size of the sample obtained by this method was larger than the average grain size of samples sintered by the conventional method with a similar heating process. 相似文献
6.
Hidehiro Yoshida Koji Morita Byung-Nam Kim Keijiro Hiraga Masayasu Kodo Kohei Soga Takahisa Yamamoto 《Journal of the American Ceramic Society》2008,91(5):1707-1710
We investigated the densification of undoped, nanocrystalline yttria (Y2 O3 ) powder by spark plasma sintering (SPS) at sintering temperatures between 650°C and 1050°C at a heating rate of 10°C/min and an applied stress of 83 MPa. In spite of the low sinterability of the undoped Y2 O3 , a remarkable densification of the powder started at about 600°C, and a theoretical density of more than 97% was achieved at a sintering temperature of 850°C with a grain size of about 500 nm. The low temperature SPS is effective for fabricating dense Y2 O3 polycrystals. 相似文献
7.
Shun J. Wu Lutgard C. De Jonghe Mohamed N. Rahaman 《Journal of the American Ceramic Society》1996,79(8):2207-2211
The sintering of ultrafine γ-Al2 O3 powder (particle size ∼10–20 nm) prepared by an inert gas condensation technique was investigated in air at a constant heating rate of 10°C/min. Qualitatively, the kinetics followed those of transition aluminas prepared by other methods. Measurable shrinkage commenced at ∼ 1000°C and showed a region of rapid sintering between ∼1125° and 1175°C followed by a transition to a much reduced sintering rate at higher temperatures. Starting from an initial density of ∼0.60 relative to the theoretical value, the powder compact reached a relative density of 0.82 after sintering to 1350°C. Compared to compacts prepared from the as-received powder, dispersion of the powder in water prior to compaction produced a drastic change in the microstructural evolution and a significant reduction in the densification rate during sintering. The incorporation of a step involving the rapid heating of the loose powder to ∼1300°C prior to compaction (which resulted in the transformation to α-Al2 O3 ) provided a method for significantly increasing the density during sintering. 相似文献
8.
Gui-hua Peng Min Liang Zhen-hua Liang Qing-yu Li Wen-lan Li Qian Liu 《Journal of the American Ceramic Society》2009,92(9):2122-2124
Silicon nitride ceramics were prepared by spark plasma sintering (SPS) at temperatures of 1450°–1600°C for 3–12 min, using α-Si3 N4 powders as raw materials and MgSiN2 as sintering additives. Almost full density of the sample was achieved after sintering at 1450°C for 6 min, while there was about 80 wt%α-Si3 N4 phase left in the sintered material. α-Si3 N4 was completely transformed to β-Si3 N4 after sintering at 1500°C for 12 min. The thermal conductivity of sintered materials increased with increasing sintering temperature or holding time. Thermal conductivity of 100 W·(m·K)−1 was achieved after sintering at 1600°C for 12 min. The results imply that SPS is an effective and fast method to fabricate β-Si3 N4 ceramics with high thermal conductivity when appropriate additives are used. 相似文献
9.
Frank J. T. Lin Lutgard C. de Jonghe Mohamed N. Rahaman 《Journal of the American Ceramic Society》1997,80(11):2891-2896
The effect of an initial coarsening step (50-200 h at 800°C) on the subsequent densification and microstructural evolution of high–quality compacts of undoped and MgO–doped Al2 O3 has been investigated during fast–firing (5 min at 1750°C) and during constant–heating–rate sintering (4°C/min to 1450°C). In constant–heating–rate sintering of both the undoped and MgO–doped Al2 O3 , a refinement of the microstructure has been achieved for the compact subjected to the coarsening step. A combination of the coarsening step and MgO doping produces the most significant refinement of the microstructure. In fast–firing of the MgO–doped Al2 O3 , the coarsening step produces a measurable increase in the density and a small refinement of the grain size, when compared with similar compacts fast–fired conventionally (i.e., without the coarsening step). This result indicates that the accepted view of the deleterious role of coarsening in the sintering of real powder compacts must be reexamined. Although extensive coarsening after the onset of densification must be reduced for the achievement of high density, limited coarsening prior to densification is beneficial for subsequent sintering. 相似文献
10.
Nobuyasu Mizutani Chung-Hsin Lu Kuzuo Shinozaki Masanori Kato 《Journal of the American Ceramic Society》1990,73(5):1214-1220
A high-temperature liquid phase (rather than a low-temperature liquid phase at 690°C as reported recently) has been demonstrated to form at 860°C on heating and to solidify at 840°C on cooling in PbFe2/3 O3 . This liquid phase not only promotes densification, but also induces the formation of rounded PbFe2/3 W1/3 O3 grains during sintering at 870°C. Through slow cooling at a rate of 25°C/h after sintering, platelike grains, designated G phase, are found to form in a thin surface layer of specimens. This formation of platelike G phase is considered to be related to the solidification and recrystallization of the liquid phase exuded from the interior. The amount of the G phase on the surfaces decreases with the increase of cooling rates, indicating that fast cooling will lead the liquid phase to be solidified in the bulk of specimens. These results reveal that the microstructure of PbFe2/3 W1/3 O3 is greatly affected by the high-temperature liquid phase; additionally, the slow cooling treatment seems to be a direct and effective method for removing the residual liquid phase from PbFe2/3 W1/3 O3 . 相似文献
11.
Preparation of Titanium Nitride/Alumina Laminate Composites 总被引:2,自引:0,他引:2
Jing-Xian Zhang Zheng-Ren Huang Dong-Liang Jiang Shouhong H. Tan Zhijian Shen Mats Nygren 《Journal of the American Ceramic Society》2002,85(5):1133-1138
A preparation route for TiN/Al2 O3 laminate composites has been described. A water-based process using Al2 O3 and TiN slurries with solids contents of 40 and 35 vol%, respectively, was used to make TiN and Al2 O3 tapes. The removal of the binder was monitored by weight-loss measurements in a thermogravimetry unit. Bodies composed of Al2 O3 and TiN tapes were densified at temperatures of 1400° and 1500°C using the Spark Plasma Sintering® (SPS) technique. Densities of >98% of the theoretical densities were approached. Crack-free and almost fully densified TiN/Al2 O3 compacts were prepared by heating the burned-out green bodies to the final sintering temperature (1500°C) at a rate of 100°C/min, and with a holding time of 5–10 min, under a pressure of 75 MPa. The microstructures of the obtained compacts were studied using scanning electron microscopy. Grain sizes in the sintered Al2 O3 and TiN compacts were similar to those of the precursor powders. Hardness and indentation fracture toughness were measured at room temperature, and the monolithic compacts as well as the laminate composites exhibited anisotropic mechanical behavior; i.e., the cracks propagated much more easily in a direction parallel to the laminas than perpendicular to them. 相似文献
12.
Effect of Heating Rate on the Sintering Behavior and the Piezoelectric Properties of Lead Zirconate Titanate Ceramics 总被引:3,自引:0,他引:3
The effect of heating rate on the sintering behavior and the piezoelectric properties of lead zirconate titanate (PZT) ceramics was investigated. Two different types of PZT (pure and doped with Nb2 O5 ) were sintered at 1150°C for 2 h with a wide range of heating rate (0.5°–100°C/min). The densification of pure PZT was improved significantly by increasing the heating rate. The improvement was attributed to the suppression of PbO volatilization and grain coarsening during heating. In contrast, the densification behavior of a PZT specimen doped with Nb2 O5 was not much influenced by the heating rate. These densification behaviors affected the piezoelectric properties of the specimens. The piezoelectric properties of pure PZT were enhanced significantly by increasing the heating rate, while those of doped specimens were improved only moderately. 相似文献
13.
Low-Temperature Sintering and Microwave Dielectric Properties of Anorthite-Based Glass-Ceramics 总被引:6,自引:0,他引:6
Chung-Lun Lo Jenq-Gong Duh Bi-Shiou Chiou Wen-Hsi Lee 《Journal of the American Ceramic Society》2002,85(9):2230-2235
TiO2 nucleated anorthite-based glass-ceramics were fabricated from glass powders. After sintering and crystallization heat treatment, various physical properties, including apparent bulk density and water absorption, were examined to evaluate the sintering behavior of anorthite-based glass-ceramic. Results showed that the complete-densification temperature for specimens was as low as 900°C. Sufficient crystallization was achieved by subsequently raising the firing temperature to 950°C, and the dielectric quality factor was promoted to the maximum value. Contents of nucleating agent (TiO2 ) played an important role in the dielectric constants. The crystallinity was controlled by raising the firing temperature at a constant heating rate. The degree of crystallization affected the dielectric properties of sintered glass-ceramics. At the resonant frequency of 10 GHz, anorthite glass-ceramics with 5 wt% TiO2 possessed the lowest permittivity of 8 and exhibited appropriate dielectric properties as compared with those with B2 O3 and 10 wt% TiO2 . 相似文献
14.
New Strategies for Preparing NanoSized Silicon Nitride Ceramics 总被引:2,自引:0,他引:2
Xin Xu Toshiyuki Nishimura Naoto Hirosaki Rong-Jun Xie Yinchun Zhu Yoshinobu Yamamoto Hidehiko Tanaka 《Journal of the American Ceramic Society》2005,88(4):934-937
We report the preparation of nanosized silicon nitride (Si3 N4 ) ceramics via high-energy mechanical milling and subsequent spark plasma sintering. A starting powder mixture consisting of ultrafine β-Si3 N4 and sintering additives of 5-mol% Y2 O3 and 2-mol% Al2 O3 was prepared by high-energy mechanical milling. After milling, the powder mixture was mostly transformed into a non-equilibrium amorphous phase containing a large quantity of well-dispersed nanocrystalline β-Si3 N4 particles. This powder precursor was then consolidated by spark plasma sintering at a temperature as low as 1600°C for 5 min at a heating rate of 300°C/min. The fully densified sample consisted of homogeneous nano-Si3 N4 grains with an average diameter of about 70 nm, which led to noticeable high-temperature ductility and elevated hardness. 相似文献
15.
Koji Watari Maria Cecilia Valecillos Manuel E. Brito Motohiro Toriyama Shuzo Kanzaki 《Journal of the American Ceramic Society》1996,79(12):3103-3108
Small amounts of Li2 O result in sintering in the AIN-Y2 O3 -CaO and AIN-CaO systems at firing temperatures <1600°C. The effect is ascribed to reduction of the liquidus temperature. Furthermore, Li2 O is removed by volatization at temperatures from 1300° to 1600°C, and its content decreases several ppm from the initial 0.3 wt%. Li2 O-doped AIN specimens containing Y2 O3 and CaO additives are well densified by firing at 1600°C for 6 h, and their thermal conductivity is 135 W. m−1. K−1 .The effect of Li2 O addition on sintering and thermal conductivity also is discussed through thermo-dynamic considerations. 相似文献
16.
Mehmet A. Akbas Michael A. McCoy William E. Lee 《Journal of the American Ceramic Society》1995,78(9):2417-2424
The early stages of sintering of lead lanthanum zirconate titanate (PLZT) 9/65/35 † ceramics prepared with 10 wt% excess PbO were monitored by quenching uniaxially pressed pellets after a variety of heat treatments. TEM revealed a PbO-rich amorphous film covering the particle surfaces and interparticle porosity in pellets quenched after 5 min at 1125° to 1180°C. This amorphous phase is indicative of the presence of a high-temperature liquid phase with composition approximately Pb0.87 Zr0.15 Ti0.04 O1.19 . The liquid composition moves toward the PbO-TiO2 eutectic as sintering progresses. After 10 to 30 min at 1180°C, the liquid composition was approximately Pb0.9 Zr0.04 Yi0.06 Ol.1 and crystallized on quenching. High densities of dislocations with = 1/2〈110〉 and low-angle boundaries were observed in samples quenched from 1180°C after 10 to 30 min. Mechanisms for the formation of these dislocations are suggested. 相似文献
17.
Composite powders, prepared by coating coarse ZrO2 particles with fine Al2 O3 powder using a chemical precipitation technique, were compacted and sintered freely at a constant heating rate of 4°C/min to ∼1600°C. Composites containing up to ∼30 vol% inclusions were sintered to nearly full density under the same conditions used for the unreinforced matrix. Furthermore, the sintering kinetics were not influenced significantly by the inclusion volume fraction. The sinterability of the composites formed from the coated powders was significantly better than that for similar composites formed from mechanically mixed powders. The present data provide a further demonstration that the use of coated powders may have widespread applicability for the fabrication, by free sintering, of dense ceramic particulate composites. 相似文献
18.
Influence of Copper(II) Oxide Additions to Zinc Niobate Microwave Ceramics on Sintering Temperature and Dielectric Properties 总被引:6,自引:0,他引:6
Dong-Wan Kim Kyung Hyun Ko Kug Sun Hong 《Journal of the American Ceramic Society》2001,84(6):1286-1290
The effect of CuO additions on the firing temperature of ZnNb2 O6 ceramics was investigated using dilatometry, transmission electron microscopy, and X-ray diffractometry. A 5 wt% CuO addition to ZnNb2 O6 ceramics significantly lowered the firing temperature from 1150° to ∼900°C. The presence of a CuO-rich intergranular phase in the specimen was observed and was evidence of the formation of a liquid phase during sintering. The composition of the liquid phase was (ZnCu2 )Nb2 O8 . In particular, the low-fired ZnNb2 O6 ceramics had good microwave dielectric characteristics— Q × f = 59 500, ɛr = 22.1, τf =–66 ppm/o C. These properties were correlated with the formation of a second phase, (ZnCu2 )Nb2 O8 . 相似文献
19.
D. Kralj B. Matkovi R. Trojko J. F. Young C. J. Chan 《Journal of the American Ceramic Society》1986,69(8):170-C
β-Ca2 Si04 can be obtained from a mixture ofCaC2 O4 -H2 O and amorphous silica by firing at 950°C as opposed to a normal sintering temperature around 1450°C. If CaCO3 is used instead of CaC2 O4 ·H2 O, four repeated firings under CO2 atmosphere are needed to obtain β-Ca2 SiO4 . The role of CO2 atmosphere during firing and the influence of specific surface of reactanm on the rate of reaction are discussed. 相似文献
20.
Two lithium-doped sialon ceramics were densified and superplastically deformed by spark plasma sintering (SPS). Rapid densification with linear shrinkage rates of approximately 5 × 10−3 s−1 were observed for samples heated at a rate of 100°C/min up to ∼1400°C under a uniaxial pressure of 40 MPa. Isothermal deformation by SPS-preprepared, fully densified ceramics performed at T ≥ 1450°C yielded strain rates in the order of 10−2 s−2 . It is suggested that a high heating rate promotes material transport via formation of a nonequilibrated oxygen-rich liquid of low viscosity. This finding most likely holds true for other liquid-phase sintered ceramics as well and has implications for cost-effective manufacturing of ceramic components. 相似文献