Grain evolution of boron carbide ceramic powder during isothermal sintering process was in situ investigated by synchrotron radiation X-ray computed tomography (SR-CT) technique. The process of grain growth and material migration during three sintering stages was clearly distinguished from the 2-D and 3-D reconstructed images. The results show that from room temperature to 1 200 ℃ (0-270 min), grains gradually approach each other and form the sintering neck but grain growth does not start, which is indicated as the initial sintering stage. While the sintering time is between 270-390 min (temperature is 1 200 ℃), material migration between grains starts, while grains and sintering neck grow up, which is defined as the middle sintering stage. As the sintering time exceeds 390 min (temperature is 1 200 ℃), pores become isolated and spheroidized, which shows the final sintering stage. The double logarithm curve of mean grain radius and time logarithm during middle stage of isothermal sintering process is obtained from reconstructed images and the grain growth exponent is 0.364 03, falling in the predicted range of the traditional sintering theory. The experiment results are in accordance with those of the traditional sintering theory and provide effective experimental data for further analysis of the sintering process and the mechanical characteristics of ceramics.
Microwave sintering is being developed as a novel technique for the preparation of dense structural ceramics,but the mature theory has not been established due to the technical difficulties.The synchrotron radiation X-ray computed tomography(SR-CT) technique was introduced for the first time into the study of microwave sintering to in-situ observe the microstructure evolution of silicon carbide(SiC) material in this paper.By applying the SR-CT technique,the reconstructed 2D and 3D images of the specimen were obtained and the double logarithm curve of mean neck size and time(Ln(x)-Ln(t)) were obtained from these reconstructed images.Various sintering phenomena including sintering neck growth during microwave treatment were observed from the reconstructed images.Furthermore,the differences in microstructure evolution and sintering kinetics between microwave and conventional sintering were analyzed based on the reconstructed images and the Ln(x)-Ln(t) curve.1) The sharp surface of grains near the contact region distinctly grew blunt and the sintering neck growth between these grains were obviously observed at the early stage.Besides,the larger particles grew faster than smaller ones.The main reason for these phenomena may be the micro-focusing effect of electric fields.2) During each of the three sintering stages,the sintering kinetics curve of double logarithm relationship between mean neck size and time shows a good linear relationship,but at the middle stage the slope of the curve increases dramatically,which is quite larger than conventional sintering.The preliminary interpretation for these extraordinary phenomena has been discussed in details.
LI YongCunXU FengHU XiaoFangQU HongYanMIAO HongZHANG ZhongXIAO TiQiao
