Production of α-Fe 2O 3 powder material with multilevel gradient porosity

A. P. Demirov, I. V. Blinkov, D. Kuznetsov, K. Kuskov, E. Kolesnikov, A. Sedegov
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Abstract

The paper studies methods for obtaining a multilevel gradient porous material by the layer-by-layer sintering of distributed α-Fe2O3 nanopowders and submicron powders. Nanopowders with an average particle size of 12 nm were obtained by the coprecipitation method, and submicron powders, which are hollow spheres, were obtained using the spray pyrolysis method. Powders were consolidated by sintering in a muffle furnace, hot pressing, and spark plasma sintering (SPS) at various temperatures, loads, and holding times. It was shown that muffle furnace sintering and hot pressing methods cannot provide a compact of enough strength due to the different activity of nanopowders and submicron powders. Powder materials were obtained by spark plasma sintering when holding at 700, 750, 800, and 900 °С for 3 min. It was found that a series of samples obtained by SPS at 750 °С has sufficient strength and open porosity of 20 % with a total porosity of 37 %. Rising temperature in this method leads to an increase in the particle size in the nanopowder volume to a micron size and partial destruction of hollow submicron spheres. It was found during the study that the phase composition of samples obtained is identical to the phase composition of initial powders. However, for a series of samples obtained by hot pressing and SPS in the nanopowder volume, there is a directed growth of crystals towards the highest electrical and thermal conductivity [001] along the punch axis. This is due to the temperature gradient between the powder volume and punches and the lowest value of the plane surface energy (110), which includes direction [001].
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本文研究了α-Fe2O3分布纳米粉体和亚微米粉体逐层烧结制备多级梯度多孔材料的方法。共沉淀法得到平均粒径为12 nm的纳米粉体,喷雾热解法得到中空球体亚微米粉体。粉末通过在马弗炉中烧结、热压和火花等离子烧结(SPS)在不同温度、负载和保温时间下进行固结。结果表明,由于纳米粉体和亚微米粉体的活性不同,采用马弗炉烧结和热压的方法无法获得足够强度的致密体。在700°、750°、800°和900°С下保温3 min得到的粉末材料,发现在750°С下SPS得到的一系列样品具有足够的强度和20%的开孔率,总孔隙率为37%。在这种方法中,温度升高会导致纳米粉末体积中的颗粒尺寸增加到微米大小,并导致空心亚微米球体的部分破坏。在研究过程中发现,所得样品的相组成与初始粉末的相组成相同。然而,对于通过热压和SPS在纳米粉末体积中获得的一系列样品,晶体沿着冲孔轴向最高的电导率和导热率定向生长[001]。这是由于粉末体积和冲头之间的温度梯度以及平面表面能的最低值(110),其中包括方向[001]。
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