Proszki azotku glinu można wytwarzać na drodze samorozwijającej się syntezy wysokotemperaturowej (SHS) z udziałem glinu i azotu, ale wysoka temperatura tej reakcji powoduje topnienie i/lub odparowanie części metalu, a w konsekwencji niską wydajnością procesu. Obecność łatwo rozkładającej się soli nieorganicznej w wyjściowej mieszaninie może zmniejszyć temperaturę układu utrudniając topienie i koalescencję ziaren glinu, a także ułatwić wnikanie azotu do wnętrza złoża proszkowego. Mieszaniny proszku glinu z różnymi ilościami prostych soli amonowych: chlorku, węglanu i azotanu poddano reakcji SHS pod ciśnieniem azotu równym 0,1 MPa lub 1 MPa. Proszki po reakcji składały się z azotku glinu, nieprzereagowanego glinu, a w niektórych przypadkach tlenoazotku glinu i korundu. Na optymalne warunki syntezy azotku glinu wpływają takie czynniki jak ilość soli - jej wzrost prowadzi do spadku temperatury układu, ciśnienie azotu - wyższe ciśnienie prowadzi do wzrostu temperatury reakcji, a także obecność tlenu w układzie.
EN
Powders of aluminium nitride can be prepared by self-propagating high-temperature synthesis (SHS) between aluminium and nitrogen but its high exothermic effect causes melting and/or evaporation of aluminium and low efficiency of such reaction. A presence of inorganic salt in the starting powder mixture can decreases a heat evolved in the SHS reaction, hinders melting and coalescence of aluminium, and helps penetration of nitrogen into interior of a powder bed. Mixtures of alumina powder and different amounts of some easy decompose ammonium salts were subjected to the SHS reaction under 0.1 or 1 MPa nitrogen. The powders were composed of aluminium nitride, unreacted aluminium and in some cases aluminium oxynitride and corundum. Different factors influence an optimum conditions for the AlN synthesis: the amount of salt, which increase leads to a decrease temperature of the system, the nitrogen pressure, the higher the pressure the higher the reaction temperature, and the presence of oxygen in the system.
High purity, fine crystalline, degradation-free at low temperature powders have attracted special interest in CAD/CAM prosthetic dentistry full ceramic restorations. This study reports the preparation and characterisation of zirconia-ceria (0.9ZrO20.1CeO2) powders. Materials were obtained from zirconium-n-alkoxide and cerium nitrate hexahydrate in the pH 2–4 and 8–10. Methods: Zirconia-ceria powders were obtained with the sol-gel method in a humid-free environment. Thermal analysis (TGA/DTA) of the as-prepared materials was made for an assessment of its behaviour at elevated temperatures. Specimens were dried at 80°C and calcinated in two stages: at 300°C with soaking time 2.5 h and 850°C with holding time 2.5 h, in order to evaluate the phase transformations. Thermal analyses of the as-dried powders were made for an assessment of its thermal behaviour during heat treatment up to 1000 °C. By X-ray diffraction (XRD), polymorphs of ZrO2 were identified. Additionally, scanning electron microscopy (SEM) and laser particle size distribution (PSD) were involved for characterisation of morphology of the powders. Results: We found a correlation between the pH of the colloidal system and the morphology of the as-obtained powders. Based on analysis (SEM,PSD), structures were identified known as soft and hard agglomerates. Conclusions: In summary, it can be stated differences were found between powder morphology depending on the used pH, which can be crucial for powder densification during sintering and compacting green bodies which, as a consequence, may be crucial for the lifetime of zirconia prostheses. Correlations between phase composition and pH are difficult to grasp, and require further more sophisticated studies.
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