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Particle size analysis and characterization of nanodiamond dispersions in water and dimethylformamide by various scattering and diffraction methods
Journal of Nanoparticle Research ( IF 2.5 ) Pub Date : 2020-01-16 , DOI: 10.1007/s11051-020-4755-3
Tomáš Kovářík , Petr Bělský , David Rieger , Jan Ilavsky , Věra Jandová , Michael Maas , Pavol Šutta , Michal Pola , Rostislav Medlín

Over the past few decades, detonation nanodiamonds (NDs) have gained increased attention due to their unique physicochemical properties. Various methods for preparation of ND suspensions have been introduced. This paper presents thermally annealed nanodiamonds dispersed via sonication and separated by centrifugation in deionized water and dimethylformamide in five weight concentrations ranging from 0.05 to 1 wt%. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were applied to study the thermal behavior of NDs. Crystallographic properties of air-annealed and dispersed NDs were examined by means of X-ray diffraction (XRD). Nanodiamond dispersions were analyzed by static light scattering (SLS), dynamic light scattering (DLS), ultra-small- and small-angle X-ray scattering (USAXS/SAXS), and high-resolution transmission electron microscopy (HRTEM). SLS and DLS give similar results of ND aggregates mean size between ~ 61 and 73 nm, regardless of solvent type and nanoparticle concentration. For dispersions with increasing concentrations of NDs, neither increased aggregate size nor different kinetics of separation during sonication and centrifugation were observed. USAXS/SAXS provided the aggregates size (2Rg) in the range from 57 to 65 nm and size of primary particles from 5.4 to 5.8 nm. HRTEM also showed presence of larger aggregates with tens of nanometers in size in both water and DMF dispersions, and size of primary particles ranging from 5.5 to 6 nm in very good agreement with SAXS.

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中文翻译:

通过各种散射和衍射方法对纳米金刚石在水和二甲基甲酰胺中的分散体进行粒度分析和表征

在过去的几十年中,爆轰纳米金刚石(NDs)由于其独特的理化性质而受到越来越多的关注。已经介绍了制备ND悬浮液的各种方法。本文介绍了通过超声处理分散的热退火纳米金刚石,并通过在去离子水和二甲基甲酰胺中离心分离得到了5种重量浓度从0.05到1 wt%的纳米金刚石。用热重分析(TGA)和差示扫描量热法(DSC)研究ND的热行为。通过X射线衍射(XRD)检查了空气退火和分散的ND的晶体学性质。通过静态光散射(SLS),动态光散射(DLS),超小和小角度X射线散射(USAXS / SAXS)对纳米金刚石分散体进行分析,和高分辨率透射电子显微镜(HRTEM)。SLS和DLS给出类似的ND结果聚集体的平均粒径在〜61至73 nm之间,与溶剂类型和纳米颗粒浓度无关。对于具有增加的NDs浓度的分散体,在超声和离心过程中既没有观察到聚集体尺寸的增加,也没有观察到不同的分离动力学。USAXS / SAXS提供的聚集体尺寸(2 R g)在57至65 nm之间,一次颗粒的尺寸在5.4至5.8 nm之间。HRTEM还显示出在水和DMF分散体中都存在数十纳米大小的较大聚集体,并且初级粒子的大小在5.5至6 nm之间,与SAXS非常吻合。

更新日期:2020-01-16
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