Triaxial porcelains are complex ceramic materials consisting of glass and crystalline phases (mainly mullite) produced from a mixture of clay, feldspar and quartz, fired at about 1300ºC (1, 2). Potash feldspars (microcline and orthoclase) are common fluxes and usually appears associated with plagioclases.
This paper concerns the crystallite size and shape evolution of mullite by firing triaxial compositions at different temperature and with different fluxing agent (K-feldspar or Li bearing petalite).
Two compositions were studied: 14% quartz, 53% kaolin, 33% K-feldspar (MGS) and 14% quartz, 53% kaolin, 33% Li-feldspar (MGC). Firing conditions were: heating ratio 2ºC/min , 180 min at T max and different (T ºC max, rising time in minutes) respectively: 1270, 815 (L1), 1300, 830 (L2), 1320, 840 (L3) and 1340, 860 (L4).
X Ray diffraction patterns of powdered samples were obtained in a Bruker D5005 diffractometer in the range 10–110 º (2 theta) at scan step ( 0.02 º ,20 sec). Complementary SEM observations of fired samples, were made in an Hitachi S-4100 microscope.
Crystallite size and shape were obtained by the Kojdecki method (3,4,5) using LaB6 (NIST SRM660a) as standard. The Table includes the obtained shape and size data for modelation of prism crystallite shape The parameter C/A, is almost constant in MGS samples but not in MGC samples where the higher size the higher C/A value, so there is a preferred crystallite growth from 1300 to 1340ºC .
The difference between the evolution of crystallite growth in MGC respect MGS compositions is in agreement with the morphologies observed by SEM (greater development of mullite.
Sample A (Å) B(Å) C (Å) C/A V 1/3
MGCL1 442 450 762 1,724 533
MGCL2 387 395 1010 2,610 536
MGCL3 488 496 1180 2,418 659
MGCL4 690 704 2196 3,183 1022
MGSL1 441 450 913 2,070 566
MGSL2 428 436 836 1,953 538
MGSL3 503 512 772 1,535 584
MGSL4 414 422 753 1,819 508
In K-feldspar formulation (MGS) there is no size growth for mullite crystallites with increasing temperature, while in petalite formulations the higher temperature the bigger crystallite sizes. Moreover different features have been found for crystallite growth in this case at highest temperature respect to that found in simple sintering or reactive sintering, with clear decrease for C/A shown at 1300ºC (5) whereas slight increases are found for mullites obtained from 3:2 gels in the range 1300-1500ºC (6).
References
1 Norton, F.H. (1988) Fine Ceramics: Technology and Applications. McGraw-Hill Inc. New York.
2. Kingery, W.D. (1976) Introduction to Ceramics. Wiley. New York.
3. Kojdecki, M. A. (2001) Mater. Sci. Forum, 378–381, 12–17
4. Kojdecki, M. A (2004) Mater. Sci. Forum, 443-444, 107-110
5. Kojdecki, M. A., Bastida, J., Serrano, F. J. & Clausell, J. V. (2001) Mater. Sci. Forum, 378–381, 747–752
6. Kojdecki, M. A., Ruiz de Sola E, Serrano F.J; Delgado Pinar V, Raventós M, Esteve V.J (2007) J. Appl. Cryst. 40, 260–276
Acknowledgements. Generalitat Valenciana project: No GV02-527. |