Trusova Elena A, Trutnev Nikolai S
Institution of Russian Academy of Sciences, A.A. Baikov Institute of Metallurgy and Materials Science, 49 Leninsky Pr., Moscow 119334, Russian Federation.
Moscow Polytechnic University, 38 Bolshaya Semenovskaya Str., Moscow 107023, Russian Federation.
Beilstein J Nanotechnol. 2018 Jun 12;9:1755-1763. doi: 10.3762/bjnano.9.166. eCollection 2018.
In the present investigation, the cryochemical approach was used for the improved synthesis of nanocrystalline metal oxides (e.g., NiO, FeO, CeO) and NaNO salt. It was shown that the solutions and sols can be treated with a liquid nitrogen stream (-196 °C) to increase the powder dispersity by 3-18 times and to increase their specific surface area by an order of magnitude. The proposed approach also reduces the agglomeration of the nanoparticles, and at the same time, results in NiO, FeO and CeO crystallite sizes of less than 10 nm (quantum dot size regime). The diameter of NaNO salt crystallites could also be reduced to ≤50 nm by freezing in a liquid nitrogen atmosphere, which is a significant improvement over analogous salts obtained by traditional methods (average diameter 300-1000 nm). The characterization of the obtained nanopowders was carried out using X-ray diffraction, transmission electron microscopy, surface area measurements and diffusion aerosol spectrometry (DAS). It was determined that the addition of 3-15 wt % of NaF to the NaNO solution prior to its cryogenic treatment results in a further decrease in the particle size of the obtained crystalline salt. NaF creates a protective coating with a thickness of 2-3 nm on the surface of NaNO crystallites, preventing their association. The results obtained show that the cryochemical processing of the solutions during the preparation phase of production allows nanopowders to be obtained with improved morphological and textural characteristics without significant increase in technical development costs.
在本研究中,采用低温化学方法改进纳米晶金属氧化物(如NiO、FeO、CeO)和NaNO盐的合成。结果表明,溶液和溶胶可用液氮流(-196℃)处理,使粉末分散度提高3至18倍,比表面积增加一个数量级。所提出的方法还减少了纳米颗粒的团聚,同时使NiO、FeO和CeO微晶尺寸小于10nm(量子点尺寸范围)。通过在液氮气氛中冷冻,NaNO盐微晶的直径也可减小至≤50nm,这比传统方法获得的类似盐(平均直径300 - 1000nm)有显著改进。使用X射线衍射、透射电子显微镜、表面积测量和扩散气溶胶光谱法(DAS)对所得纳米粉末进行表征。确定在低温处理之前向NaNO溶液中添加3 - 15wt%的NaF会导致所得结晶盐的粒径进一步减小。NaF在NaNO微晶表面形成厚度为2 - 3nm的保护涂层,防止它们聚集。所得结果表明,在生产制备阶段对溶液进行低温化学处理能够获得具有改进的形态和结构特征的纳米粉末,而不会显著增加技术开发成本。