Dynamic strength of fine-grained alumina ceramics obtained by Spark Plasma Sintering

N. Melekhin, M. Boldin, А. Popov, А. Bragov, А. R. Filippov, S. Shotin, A. Murashov, A. Nokhrin, V. Chuvil’deev, N. Tabachkova
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Abstract

The results of dynamic compressive testing of alumina samples with different grain sizes sintered from nano and fine α-Al2O3 powders are presented. The ceramics were obtained by spark plasma sintering (SPS). The effect of heating rate (Vh), sintering temperature (Ts), holding time (ts), cooling rate (Vc) on hardness, fracture toughness, dynamic strength stress (σY) of Al2O3 has been studied. An amorphous layer of nanometer thickness was present on the surface of nanopowders in the initial state. After sintering, the grain boundaries of the ceramics had a crystalline structure; no inclusions of the amorphous phase were found. It has been suggested that during the SPS process, an amorphous structure containing an excess free volume is transformed into a crystalline phase with the formation of dislocation-type defects at the grain boundaries, which create long-range internal stress fields. It is shown that nanopores less than 50 – 100 nm in size are present at the grain boundaries of sintered ceramics. It is shown that the nonmonotonic nature of the dependence of σY on the temperature and time of the SPS is due to the simultaneous change in the density, the nonequilibrium state of the grain boundaries, and the grain size of the ceramic. It is shown that a decrease in the degree of nonequilibrium of the grain boundaries of alumina due to an increase in the SPS temperature or an increase in the holding time makes it possible to increase the dynamic strength of alumina. It has been established that an increase in the cooling rate leads to the formation of compressive residual stresses and a slight increase in σY of ceramics. The maximum dynamic strength (σY = 1755 MPa) for alumina ceramics with average grain size 1.6 – 2 µm obtained by SPS (Vh = 50 °С/min, Ts = 1520 °С, ts = 50 min).
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火花等离子烧结获得细晶氧化铝陶瓷的动态强度
介绍了纳米α-Al2O3粉末和细α-Al2O3粉末烧结不同晶粒度氧化铝试样的动态压缩试验结果。采用火花等离子烧结(SPS)法制备陶瓷。研究了加热速率(Vh)、烧结温度(Ts)、保温时间(Ts)、冷却速率(Vc)对Al2O3硬度、断裂韧性、动强度应力(σY)的影响。在初始状态下,纳米粉体表面存在一层纳米厚度的非晶层。烧结后,陶瓷的晶界呈结晶结构;未发现非晶相夹杂物。在SPS过程中,含有过量自由体积的非晶态结构转变为晶相,在晶界处形成位错型缺陷,形成长范围内应力场。结果表明,烧结陶瓷的晶界上存在着尺寸小于50 ~ 100 nm的纳米孔。结果表明,σY对SPS温度和时间的非单调性是由于密度、晶界非平衡态和晶粒尺寸同时发生变化所致。结果表明,SPS温度的升高或保温时间的延长会降低氧化铝晶界的非平衡程度,从而有可能提高氧化铝的动态强度。结果表明,随着冷却速率的增大,陶瓷的残余压应力逐渐形成,σY值略有增大。SPS (Vh = 50°С/min, Ts = 1520°С, Ts = 50 min)得到平均晶粒尺寸为1.6 ~ 2µm的氧化铝陶瓷的最大动态强度(σY = 1755 MPa)。
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