以乙酸锰(Mn(Ac)2·4H2O)、双氧水(H2O2)及氨水(NH3·H2O)为原料,通过水浴化学沉淀直接合成Mn3O4纳米粉体.采用XRD和SEM对样品成分和形貌进行表征,发现水浴温度80℃、原料物质的量比为1∶2∶2时合成的样品结晶完善,形状规则,尺寸均匀.双氧水用量较少时有异形结构生成;氨水不足会造成产物大小不均匀;水浴温度过高或过低都会造成产物形状不规则,粒径分布变宽.TG/DTA结果显示,样品在空气中升温时存在3次转变,分别在202℃、338℃附近生成了相似结构的Mn3O4,仅晶格尺寸发生变化;超过455℃生成了立方方铁锰矿的α-Mn2O3.对比产物在不同温度下煅烧后的XRD图谱和TEM照片,发现600℃煅烧生成的α-Mn2O3结晶完善,团聚较少,晶格尺寸(a=b=c=9.412(A))接近标准值.
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