Pulse Plasma Sintering of NiAl-Al2O3 Composite Powder Produced by Mechanical Alloying with Contribution of Nanometric Al2O3 Powder

NiAl-Al2O3 composites, fabricated from the prepared composite powders by mechanical alloying and then consolidated by pulse plasma sintering, were presented. The use of nanometric alumina powder for reinforcement of a synthetized intermetallic matrix was the innovative concept of this work. Moreover, this is the first reported attempt to use the Pulse Plasma Sintering (PPS) method to consolidate composite powder with the contribution of nanometric alumina powder. The composite powders consisting of the intermetallic phase NiAl and Al2O3 were prepared by mechanical alloying from powder mixtures containing Ni-50at.%Al with the contribution of 10 wt.% or 20 wt.% nanometric aluminum oxide. A nanocrystalline NiAl matrix was formed, with uniformly distributed Al2O3 inclusions as reinforcement. The PPS method successfully consolidated NiAl-Al2O3 composite powders with limited grain growth in the NiAl matrix. The appropriate sintering temperature for composite powder was selected based on analysis of the grain growth and hardness of Al2O3 subjected to PPS consolidation at various temperatures. As a result of these tests, sintering of the NiAl-Al2O3 powders was carried out at temperatures of 1200 °C, 1300 °C, and 1400 °C. The microstructure and properties of the initial powders, composite powders, and consolidated bulk composite materials were characterized by SEM, EDS, XRD, density, and hardness measurements. The hardness of the ultrafine-grained NiAl-Al2O3 composites obtained via PPS depends on the Al2O3 content in the composite, as well as the sintering temperature applied. The highest values of the hardness of the composites were obtained after sintering at the lowest temperature (1200 °C), reaching 7.2 ± 0.29 GPa and 8.4 ± 0.07 GPa for 10 wt.% Al2O3 and 20 wt.% Al2O3, respectively, and exceeding the hardness values reported in the literature. From a technological point of view, the possibility to use sintering temperatures as low as 1200 °C is crucial for the production of fully dense, ultrafine-grained composites with high hardness.

Characterization of Al2O3 Samples and NiAl–Al2O3 Composite Consolidated by Pulse Plasma Sintering

The paper describes an investigation of Al2O3 samples and NiAl–Al2O3 composites consolidated by pulse plasma sintering (PPS). In the experiment, several methods were used to determine the properties and microstructure of the raw Al2O3 powder, NiAl–Al2O3 powder after mechanical alloying, and samples obtained via the PPS. The microstructural investigation of the alumina and composite properties involves scanning electron microscopy (SEM) analysis and X-ray diffraction (XRD). The relative densities were investigated with helium pycnometer and Archimedes method measurements. Microhardness analysis with fracture toughness (KIC) measures was applied to estimate the mechanical properties of the investigated materials. Using the PPS technique allows the production of bulk Al2O3 samples and intermetallic ceramic composites from the NiAl–Al2O3 system. To produce by PPS method the NiAl–Al2O3 bulk materials initially, the composite powder NiAl–Al2O3 was obtained by mechanical alloying. As initial powders, Ni, Al, and Al2O3 were used. After the PPS process, the final composite materials consist of two phases: Al2O3 located within the NiAl matrix. The intermetallic ceramic composites have relative densities: for composites with 10 wt.% Al2O3 97.9% and samples containing 20 wt.% Al2O3 close to 100%. The hardness of both composites is equal to 5.8 GPa. Moreover, after PPS consolidation, NiAl–Al2O3 composites were characterized by high plasticity. The presented results are promising for the subsequent study of consolidation composite NiAl–Al2O3 powder with various initial contributions of ceramics (Al2O3) and a mixture of intermetallic–ceramic composite powders with the addition of ceramics to fabricate composites with complex microstructures and properties. In composites with complex microstructures that belong to the new class of composites, in particular, the synergistic effect of various mechanisms of improving the fracture toughness will be operated.

Evaluation of Harmonic Structure Obtained in Mechanically Milled Powders and Pulse Plasma Sintered Compacts of Austenitic Steel

The paper describes an attempt to obtain harmonic structure (HS) in AISI308L steel. Harmonic structure is the term related to the microstructure fabricated by mechanical milling of metallic powders under soft milling conditions, resulting in the formation of plastically deformed, grain-refined shell and unchanged core. This microstructure can be preserved after successful powder compaction. The powders of AISI308L steel were milled under soft condition up to 50 h and then compacted by pulse plasma sintering at 900–1100 °C. For powders and compacts XRD, SEM and hardness measurements were applied as characterization techniques. The milling process resulted in austenite transformation into nanocrystalline ferrite and formation of grain refined outer layer. The applied pulse plasma sintering parameters allowed preservation of this microstructure and manufacturing of compacts with homogeneous distribution of elements, relative density above 95% and hardness in the range 167–185 HV, depending on sintering temperature. Simultaneously, the starting phase composition was restored, i.e., austenite with 12% contribution of ferrite. The crystallite size of austenite was about 20 nm and was significantly smaller then in starting powders.

Формирование мелкодисперсного термоэлектрика Si-=SUB=-1-x-=/SUB=-Ge-=SUB=-x-=/SUB=- при электроимпульсном плазменном спекании

The kinetics of diffusion processes occurring d0uring the formation of polycrystalline Si1-xGex nanostructures (x=0.20, 0.35) by electro-pulse plasma sintering in the temperature range 20-1200°C was studied for the first time. A mechanism for the formation of a solid solution of SiGe is proposed as a result of a comprehensive study of the microstructure and phase composition of samples with particle sizes from 150 nm to 100 μm, together with the analysis of experimental sintering maps. It is based on the phenomenon of mutual diffusion of Si and Ge atoms that occurs during the entire sintering process. For the selected sintering modes, the grain size of the formed SiGe corresponds to the size of the initial powder particles.

Influence of Manufacturing Technology on the Structure of 80W–20Re Heavy Sinters

Preliminary measurement results of 80W–20Re heavy sinters are presented in this paper. Tested samples were taken from three different technology processes, i.e., resistance sintering (RS), pulse plasma sintering (PPS), and conventional sintering in a vacuum furnace. In the first two cases, the obtained sinters were of similar usable properties (porosity and microhardness), while for vacuum sintering, the material with high porosity was obtained. At the same time, it was found that sintering with the use of electric current (RS, PPS) generates microstructures with highly elongated grains.

Influence of compaction and degassing on the properties of submicron WCCo produced by the PPS method

Influence of compaction and degassing on the properties of submicron WCCo produced by the PPS method. The present study is concerned with the effect of the parameters of the degassing operation (temperature, load and heating rate) conducted at the initial stage of the Pulse Plasma Sintering (PPS) process and the sintering temperature at the final stage of the process, on the properties and microstructure of WCCo with a 6wt% cobalt content sintered by this method. The results of the study have shown that when the heating rate is too high, the material obtained is porous. In most experiments, the sintering temperature of 1050°C appeared to be too low to obtain WCCo composites with density close to the theoretical value (GT). Sintering at the temperature increased to 1070°C yielded sinters with density above 99%GT, with hardness of about 1900 HV30 and fracture toughness KIC=9.3 MNm-3/2.