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Electrosynthesis and characterization of nanocrystalline UO2 coating from aqueous alkaline electrolyte

机译：碱性电解质水溶液中纳米晶UO2涂层的电合成及表征

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In this study, UO2 coating was deposited by direct current (DC) electrolysis from an aqueous electrolyte containing UO2(NO3)(2) as source of uranium. Deposition parameters such as electrolyte pH, temperature and current density were optimized in order to obtain a smooth adherent UO2 coating on metallic substrates. The effect of pH, temperature and current density on the deposition rate and on faradic current efficiency (CE) was studied in detail. The study revealed that the control over pH of the electrolyte was more important in comparison to temperature and current density to obtain a smooth deposition of UO2 from this uranyl nitrate-oxalate complex electrolyte. Grazing incidence X-ray diffraction (GI-XRD) of the as-deposited coating with a broad peak confirmed amorphous to ultra-nanocrystalline deposition. Upon vacuum annealing at higher temperature, the as-deposited coating transformed into nanocrystalline fcc UO2 with the appearance of sharper (111), (220), (220), (222) XRD reflections. The average grain size obtained was 13.2 nm for the sample annealed at 700 degrees C. In the presence of air, the fcc UO2 coating was transformed largely into the hcp U3O8 phase with a small percentage of hcp UO3 at temperatures higher than 400 degrees C. The surface morphology of the as-deposited coating showed a granular morphology with the appearance of few cracks. Upon annealing at 700 degrees C, the film showed a network of cracks throughout the surface with numerous pores inside the UO2 matrix. Composition analysis by EDS of the film confirmed the presence of uranium and oxygen. Cross-sectional FESEM analysis of the focused ion beam (FIB) cut samples confirmed deposition of a 6 mm thick UO2 coating. Upon annealing at 700 degrees C, it converted into a highly porous UO2 coating with improved adhesion with the substrate.
机译：在该研究中，通过从含有UO 2（NO 3）（2）的水性电解质作为铀来源，通过直接电流（DC）电解沉积UO2涂层。优化沉积参数，例如电解质pH，温度和电流密度，以便在金属基板上获得平滑的粘附UO2涂层。详细研究了pH，温度和电流密度对沉积速率和法拉米电流效率（CE）的影响。该研究表明，与温度和电流密度相比，电解质对电解质的pH值更重要，以从该硝酸铀酰酯复合电解质中获得UO 2的平滑沉积。用宽峰的沉积涂层的放牧发病X射线衍射（Gi-XRD）证实了无定形的超纳米晶体沉积。在较高温度下的真空退火时，将沉积的涂层转化为纳米晶FCC UO 2，外观锐白（111），（220），（220），（222）XRD反射。在700摄氏度下，样品的平均晶粒尺寸为13.2nm。在空气存在下，将FCC UO 2涂层在很大程度上转化为HCP U3O8相，在高于400℃的温度下少量HCP UO 3。沉积涂层的表面形态显示出颗粒形态，外观少量裂缝。在700摄氏度下退火时，该薄膜在整个表面上显示了裂缝网络，在UO 2基质内部具有许多孔隙。薄膜EDS的成分分析证实存在铀和氧气。聚焦离子束（FIB）切割样品的横截面FeSEM分析证实了6mm厚的UO2涂层的沉积。在700℃下退火时，它将其转化为高度多孔的UO 2涂层，其具有改善的粘合性与基材。

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  • 来源
    《RSC Advances》 |2016年第113期|共10页
  • 作者

    Varshney J.; Rajak S.; Ghosh S. K.; Vishwanadh B.; Tewari R.; Sastry P. U.; Kain V.; Dey G. K.;

  • 作者单位

    Bhabha Atom Res Ctr Mat Proc &

    Corros Engn Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Proc &

    Corros Engn Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Proc &

    Corros Engn Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Sci Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Sci Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Solid State Phys Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Proc &

    Corros Engn Div Bombay 400085 Maharashtra India;

    Bhabha Atom Res Ctr Mat Sci Div Bombay 400085 Maharashtra India;

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  • 正文语种 eng
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