Fabrication of Silicon Nitride Nano-Ceramics by High-Energy Mechanical Milling and Spark Plasma Sintering

Author(s):  
Xin Xu ◽  
Toshiyuki Nishimura ◽  
Naoto Hirosaki ◽  
Rong Jun Xie ◽  
Yoshinobu Yamamoto
2005 ◽  
Vol 287 ◽  
pp. 166-170 ◽  
Author(s):  
Xin Xu ◽  
Toshiyuki Nishimura ◽  
Naoto Hirosaki ◽  
Rong Jun Xie ◽  
Yoshinobu Yamamoto

The fabrication of dense Si3N4 nano-ceramics via a high-energy mechanical milling process and subsequent spark plasma sintering (SPS) was reported in this paper. A thermodynamically stable β-Si3N4 powder mixed with 5-mol% Y2O3 and 2-mol% Al2O3 was used as starting powders for high-energy mechanical milling. Milling resulted in the significant decrease of crystalline size and the amorphization of the starting powders. Based on XRD measurements, the amount of the amorphous phase and the grain sizes of the remaining crystalline silicon nitride depended on the charge ratio. Milled powders could be SPSed at relatively low temperature. A homogenous dense silicon nitride ceramics with grain diameter of about 70 nm could be fabricated through SPS at a low temperature of 1600oC for 5 min. The significant decrease of grain size greatly increased the hardness of obtained ceramics.


2022 ◽  
pp. 131671
Author(s):  
Dina V. Dudina ◽  
Tatyana F. Grigoreva ◽  
Vyacheslav I. Kvashnin ◽  
Evgeniya T. Devyatkina ◽  
Sergey V. Vosmerikov ◽  
...  

2021 ◽  
Vol 21 (4) ◽  
pp. 2687-2691
Author(s):  
Nguyen Thi ◽  
Hoang Oanh ◽  
Nguyen Hoang Viet

The present work is focused on the fabrication and the investigation of microstructures of copperbased TiC nanocomposites produced by mechanical milling in a high energy planetary ball mill. TiH2, carbon and copper powders were used as starting materials in which In-Situ reaction between carbon and TiH2 occurs to form TiC nanoparticles. The mixture powders of Cu–TiH2–C were milled for 12 h at 450 rpm in Argon gas. Annealing treatment process at 950 °C for 2 h was applied for as-milled composite powders to enhance In-Situ reaction. The consolidation of composite powders was conducted by spark plasma sintering under uniaxial pressing of 70 MPa. Sintering procedure was done at 950 and 1000 °C for 5 min. The results indicated that as TiC nanoparticles are formed after sintering at 950 °C and the TiC particles are increased up at higher sintering temperature of 1000 °C. Fracture surface of sintered samples shows ductile mode. HR-TEM image showed the crystal size of copper was about 10 nm for sample sintered at 1000 °C. The hardness and relative density of the nanocomposites increase when increasing sintering temperature.


2007 ◽  
Vol 336-338 ◽  
pp. 1001-1004 ◽  
Author(s):  
Xin Xu ◽  
Toshiyuki Nishimura ◽  
Naoto Hirosaki ◽  
Rong Jun Xie ◽  
Yoshinobu Yamamoto ◽  
...  

In previous report, we succeeded in preparing dense nano-sized ceramics with the composition of Y- α-sialon (m=1.35, n=0.675) by high-energy mechanical milling followed by spark plasma sintering. The superplastic deformation of the obtained nano-ceramics was studied in this report. A good ductility of the nano-sized ceramics has been confirmed, which arised from the nano-sized grains and large amount of transient liquid phase. The effects of deformation on the phase and microstructural evolution were also studied. The nano-sized grains promoted the formation of elongated α-sialon grains during post-annealing at 1850oC for 3 h, which would strengthen and toughen the deformed ceramics.


2005 ◽  
Vol 16 (9) ◽  
pp. 1569-1573 ◽  
Author(s):  
Xin Xu ◽  
Toshiyuki Nishimura ◽  
Naoto Hirosaki ◽  
Rong-Jun Xie ◽  
Yoshinobu Yamamoto ◽  
...  

2005 ◽  
Vol 287 ◽  
pp. 156-159 ◽  
Author(s):  
Toshiyasu Nishimura ◽  
Xin Xu ◽  
Naoto Hirosaki ◽  
K. Kimoto ◽  
Yoo Yamamoto ◽  
...  

A commercial silicon nitride powder with oxide sintering additives was ground with high-energy ball mill to obtain nano-sized powder. Metallic aluminium powder was added as a grinding additive. Effect of high-energy ball milling was evaluated by X-ray diffraction analysis. After milling, height of background increased and peak height of silicon nitride decreased in XRD chart, which suggested that vitrification and/or decrease in grain size of silicon nitride occurred. The milled powders were sintered by spark plasma sintering system. Aluminium nitride was formed during sintering by reaction of aluminium and atmospheric nitrogen. Dense nano-ceramics, which were composed of silicon nitride and sialon, were obtained by sintering at 1550 oC.


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