The sequence of reactions during the synthesis of sodium niobate, potassium niobate, and sodium potassium niobate from alkaline carbonates and niobium oxide has been studied by diffusion couples in the temperature range between 500° and 700°C for up to 48 h. The reactions proceed by coupled diffusion of alkaline and oxygen ions into niobium oxide. The first phase to form at the interface Na2CO3/Nb2O5 is Na2Nb4O11 at 500°C. The perovskite phase forms only after heating at 700°C at the boundary between Na2Nb4O11 and Na2CO3. In the K2CO3/Nb2O5 diffusion couple, the sequence of phases after heating at 600°C is Nb2O5/K6Nb10.88O30/K4Nb6O17/KNbO3/K2CO3. In the (K2CO3+Na2CO3)/Nb2O5 diffusion couple the (K,Na)NbO3 solid solution forms via the intermediate phase (K,Na)2Nb4O11 at 600°C. The order of magnitude of the parabolic reaction rate constant for the diffusion‐controlled reaction at 600°C is about 10−15 m2/s for the (K2CO3+Na2CO3)/Nb2O5 and the K2CO3/Nb2O5 systems, which is about one order of magnitude less than that for Na2CO3/Nb2O5 (10−14 m2/s). The reaction rate in the ternary system is determined by the diffusion of the slower species, i.e., the potassium ions.
New lead-free relaxors have been produced from the K0.5Na0.5NbO3–SrTiO3 (KNN-STO) system. The solid solubility within the studied range of compositions (1 - x) K0.5Na0.5NbO3–xSrTiO3 was observed for x up to 0.33. A pseudo-cubic perovskite structure was determined for x = 0.15 to 0.25. The high density and the uniform distribution of fine grains and pores were confirmed by the translucency of these ceramics. The 0.85KNN-0.15STO composition reaches the dielectric permittivity of above 3000 at room temperature. Dielectric spectroscopy measurements revealed that, as with lead-based complex perovskites, the cationic distribution disorder is reflected in relaxorlike properties, thus suggesting possible applications based on this environmentally friendly lead-free ceramic system.
In this work the effect of firing temperature and firing time on the phase composition, microstructure, biaxial flexural strength, and temperature coefficient of expansion (TCE) of low‐temperature cofired ceramic (LTCC) material is presented. At temperatures around 700°C the Al2O3 starts to dissolve in a low viscosity glass phase and this takes place up to 800°C, when 10 wt% of Al2O3 ceramic filler is dissolved in the glass phase forming the alumina‐enriched area. This area is suitable for the crystallization of anorthite, which nucleates on the Al2O3 particles. The crystallization starts at 875°C and the mass fraction of anorthite increases with increasing temperature until it reaches a plateau value of around 22 wt% at higher temperatures or longer firing times. The biaxial flexural strength of the LTCC increases with increasing firing temperature from 135 MPa (at 800°C) to around 300 MPa (at 900°C). The major effect on the biaxial flexural strength of LTCC is that of porosity. The effect of the amount of anorthite on the LTCC biaxial flexural strength is minor. The TCE of the LTCC decreases from 5.6 × 10−6 to 5.0 × 10−6 K−1 with increasing firing temperatures or times and it is correlated with the anorthite mass fraction, which crystallizes at the expense of a decreasing amount of glass phase in the LTCC.
Laminated 3D structures made using lowtemperature co-fired ceramic (LTCC) technology are practical for ceramic micro-electro-mechanical systems (C-MEMS). The sensors for mechanical quantities, and/or actuators, are fundamental parts of MEMS. Thick-film resistors can be used to sense the mechanical deformations, and thick-film piezoelectric materials can be used as electro-mechanical transducers in a C-MEMS structure. The integration of these thick-film materials on LTCC substrates is in some cases difficult to realise due to interactions with the rather glassy LTCC substrates. The subject of our work is an investigation of thick-film materials for electro-mechanical transducers (sensors and actuators) and their compatibility with LTCC substrates. Resistors made with commercial thick-film resistor materials for use as sensors on LTCC substrates have been investigated and evaluated. Ferroelectric ceramic materials based on solid solutions of lead zirconate titanate (PZT) with low firing temperatures around 850°C were developed for thick-film technology and evaluated on LTCC substrates.
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