Hot-press sintering studies of amorphous silicon nitride powders

The hot-press sintering behaviour of amorphous Si₃N₄ powders prepared from the ammonia pyrolysis of polycarbosilane or hydridopolysilazane polymers was studied. In the presence of yttria and alumina, the amorphous powders sintered to > 98% of theoretical density at 2023 K. Both the microstructure and average four-point MOR bend strengths, of test bars machined from the sintered compacts were comparable to those obtained from UBE SN-E-10 Si₃N₄ powder processed under the same conditions. However, in contrast to commercial crystalline powders, between approximately 1690 and 1700 K the amorphous Si₃N₄ powders underwent a rapid shrinkage corresponding to 50–60% of the total densification. In this narrow temperature regime, a radical change in morphology and phase composition of the amorphous powder occurred. Prior to 1690 K, the Si₃N₄ powders were totally amorphous as determined by X-ray diffraction analysis and consisted of angular shards with an average particle size of 2–3 m. Samples quickly cooled after heating to 1700 K, consisted of a 53/47 mixture of equiaxed and Si₃N₄ crystallites with an average particle size of 0.1–0.3 m. Thus, the rapid densification at R~ 1700 K is identified with the amorphous to ( + ) transition. Beyond 1700 K, these samples gradually densified to the maximum density as mentioned. The fully densified samples consisted of 100% -Si₃N₄ phase.     

Microwave and conventional sintering of rapidly solidified Al2O3-ZrO2 powders

The Al₂O₃-ZrO₂ eutectic composition was rapidly solidified, forming amorphous and crystalline structures. The as-quenched material was crushed and pressed into pellets which were sintered conventionally or with microwaves. Conventional and microwave sintering at temperatures up to 1600 °C resulted in a microstructure where 100–200 nm ZrO₂ grains were present intergranularly in the -Al₂O₃ grains. Larger ZrO₂ grains (1 m) were found intergranularly. The as-quenched lamellar structure spheroidized during sintering at high temperatures. Boron contamination of the powders resulted in more homogeneous and dense as-fired samples but promoted the ZrO₂ tetragonal-to-monoclinic transformation, which was attributed to increased grain boundary diffusivity. Conventional sintering at low temperatures resulted in the formation of rods of an Al₂O₃-rich phase which grew from a low-melting B₂O₃-rich liquid.     

Microwave sintering of titanium diboride

Using a 2.45 GHz, 6 kW microwave furnace adapted for inert gas sintering, titanium diboride (TiB₂) can be rapidly microwave-sintered to >90% of theoretical density with sintering temperatures of 1900 to 2100 °C and soak times of 30 min or less. Densification behaviour with low-level additives was evaluated; 3 wt% chromium diboride (CrB₂) was an excellent sintering aid-grain growth inhibitor. A special covering system was required to produce oxidefree TiB₂. Specimen surface and interior temperatures were determined with a hole experiment. Comparison with conventional sintering indicates that microwave sintering of TiB₂-3 wt% CrB₂ occurs at lower temperatures (i.e., 200 °C lower) and can yield material with improved hardness, grain size, and fracture toughness.A portion of the material in this article was presented at a Symposium on Microwave Processing of Ceramics, 91st Annual Meeting of the American Ceramic Society, Indianapolis, Indiana, April 1989.Operated for the U.S. Department of Energy by Martin Marietta Energy Systems, Inc., under contract DE-AC05-84OR21400.     

Microwave sintering of zirconia ceramics

The potential of a microwave heating technique for the sintering of 3Y-TZP ceramics is demonstrated. High density samples were obtained by short duration firing in a domestic microwave oven. The ultrafine and monomodal size distribution of grains resulting from the process has important implications in terms of mechanical properties. The hardness and fracture toughness values compare very well with long duration, conventionally fired 3Y-TZP ceramics.     

Effects of amorphous silica coatings on the sintering behaviours of SiC whisker-reinforced Al2O3 composites

In this study, pressureless sintering of silicon carbide whisker (SiC_w)-reinforced alumina composites was investigated. SiC whiskers or Al₂O₃ powders were coated with amorphous silica, and sintering behaviour was analysed according to the powder characteristics of the composite. It was found that amorphous silica coatings improved densification as compared with uncoated powders, because the viscous flow allows the release of any tensile stress due to differential shrinkage between the matrix and the silicon carbide whiskers. Mullite occurred when amorphous silica coatings reacted with alumina at 1500 °C, which resisted the viscous sintering of the amorphous silica coatings.     

Selective laser sintering of PZT ceramic powders

Conditions for the selective laser-induced layer sintering of a stoichiometric mixture of PbO, ZrO₂, and TiO₂ powders with the formation of bulk PZT ceramic articles were studied. The laser processing allows articles of the PZT ceramics to be obtained immediately in the course of sintering or upon additional annealing. Data on the microstructure and phase composition of the synthesized PZT ceramics are presented.     

Laser synthesis of nanometric silica powders

A high power tunable continuous wave CO₂ laser was used in the synthesis of ultrafine powders. Monodisperse silica powders in the nanometric range (30 nm) were produced via ultrasonic injection of aerosol droplets into the beam of the laser. The precursor used was tetrathoxysilane which stronngly absorbs the CO₂ laser radiation at 9.3 μm. The as-formed powders were amorphous and contained free carbon (20 wt%) which was easily oxidized in air at 600°C.     

Microwave sintering of calcium phosphate ceramics

Microwave sintering of hydroxyapatite (HAP) and tri-calcium phosphate (TCP) ceramics were studied using a commercial 2.45 GHz, 3 KW fully automated microwave system. Four different powder compositions, apart from pure HAP and TCP, were prepared with small amount of different oxide additives e.g., magnesium oxide, zinc oxide and titanium oxide. All samples were densified at 1250 °C for 30 min. Sintered samples had high density and homogeneous microstructure for all compositions. Phase analysis using XRD showed no major variations from starting materials. Presence of additives increased compressive strength between 100 and 200%. Fractured surfaces showed clear signs of intergranular fracture in undoped HAP and TCP while in doped samples, fracture modes were either transgranular or mixed mode. In comparison to conventional sintering, microwave sintering of calcium phosphate ceramics was found to be economically exciting due to substantial reduction in processing time and energy expenditure due to volumetric heating of samples.     

A recipe for sintering submicron silver powders

A process for sintering submicron silver powders is described. The process allows for a reasonable surface area (determined by the BET adsorption isotherm technique) whilst maintaining a strong mechanical contact between the sinter and silver foils or silver plated copper plates.     

氧化锆纳米粉体烧结性能研究

为了研究纳米氧化锆粉体的烧结性能,以4种不同粒度的氧化锆粉体为原料,在热分析仪上测试了室温～1000℃范围内坯体的形变量和热膨胀性能.采用1450℃恒温1～6 h的烧结工艺,制备了氧化锆陶瓷,并进行了性能表征.结果表明:粉料1次粒子粒径越小,其初始烧结温度越低;粉料的团聚粒径越小,分布越窄,坯体的烧结致密化越容易.     

Direct laser sintering of a silica sand

As an application study of rapid prototyping, commercially available silica sand was successfully direct-laser-sintered in a self-developed high-temperature laser sintering equipment. The mechanism of powder-state sand becoming a solid state block during the laser sintering process was disclosed by scanning electron microscope (SEM) and energy dispersive X-ray (EDX) analysis on sand particles and sintered samples. The effect of process parameters to the accuracy, strength and surface finish of sintered parts was investigated and thus a set of optimal parameters has been obtained for the sand sintering process. The feasibility of using this material and process to build casting moulds for metal casting was also investigated and discussed.     

纳米FeNi粉体的吸波性能研究

利用液相还原法制备了纳米FeNi粉体。利用XRD和SEM分别对FeNi粉体的物相、形貌进行了分析,并通过矢量网络分析仪,利用同轴方法对FeNi粉体/固体石蜡复合材料进行了电磁参数的测定。研究表明,制备出的铁镍复合粉体主要成分为FeNi;FeNi粉体为球形,直径约为100 nm,分布均匀。利用实验所得到的数据模拟了FeNi复合材料不同厚度涂层的吸波性能,当涂层厚度为2 mm时,复合材料的吸收峰值R达到-6.25 d B,小于-4 dB带宽从13.24~16.47GHz;在2~18 GHz频率范围内,当涂层厚度为4 mm时,FeNi粉体/固体石蜡复合材料出现了两个吸收峰,其值都小于-4.5 dB。     

Crystallization kinetics of amorphous Ni78P22 powders and hydrogen adsorption on both amorphous and crystal alloy powders

A thermal and kinetic investigation of the behaviour of amorphous and crystal powder alloy Ni₇₈P₂₂ was performed in a hydrogen atomsphere. It was shown that the amorphous alloy absorbs hydrogen within the temperature range 393 to 520 K. After that it is transformed into the crystal (stable) state in two steps at 615 and 670 K, respectively, thus forming stable Ni and Ni₃P phases. The crystal form of the same sample also adsorbs hydrogen, but at lower temperatures ranging from 310 to 520 K, The activation energies of the crystallization process, as well as the frequency factors, the rate constants and the enthalpy of crystallization were determined. Both kinetic and thermal parameters of the hydrogen adsorption process taking place in at least two steps, as in the crystallization process, were also determined.