Simultaneous Sc-doping and suboxide transformation of anatase TiO2 nanoparticles

IF 5.5 2区材料科学 Q1 MATERIALS SCIENCE, CHARACTERIZATION & TESTING Materials Characterization Pub Date : 2025-02-07 DOI:10.1016/j.matchar.2025.114831

Victor Y. Zenou , Mária Čaplovičová , Martin Kormunda , Snejana Bakardjieva

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Abstract

Self-assembled agglomerates of 4 at.% Sc doped titania (4SDT) nanoparticles (NPs) were obtained using a simple water-based co-precipitation of titanium oxysulfate and scandium oxalate with urea at low temperature. Undoped samples were also prepared for comparison.

Aberration-corrected scanning transmission electron microscopy and dual electron energy loss spectroscopy (DualEELS), showed that 4SDT agglomerates comprised self-assembled anatase NPs and sub-stoichiometric trititanium pentoxide (β-Ti₃O₅). The Ti₃O₅ either surrounded the anatase NPs as an ultra-thin outer layer or grew on the anatase surface in randomly distributed “nanoislands” closely connected to the Sc³⁺ ion.

Heating to 800 °C under air caused the Sc³⁺ to segregate out the anatase lattice to form Sc-rich oxides (usually Sc₄Ti₃O₁₂). Also, it was detected that the Ti⁴⁺ amount increased at the expense of Ti³⁺.

X-ray photoelectron spectroscopy (XPS), employed to investigate the elements' surface composition, oxidation states, and electronic configurations, showed 4.6 % Sc relative to the sum of Sc and Ti, close to the nominal composition of 4 %. The O/Ti values found for 4SDT by XPS and EELS were 2.3 ± 0.1 and 2.2 ± 0.2, respectively.

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锐钛矿型TiO2纳米粒子的sc掺杂与亚氧化物转化

自组装的团块4 at。采用简单的水基低温共沉淀法将硫酸氧钛和草酸钪与尿素共沉淀法制备了% Sc掺杂二氧化钛（4SDT）纳米粒子。还制备了未掺杂样品进行比较。扫描透射电镜和双电子能量损失谱（DualEELS）显示，4SDT团聚体由自组装锐钛矿NPs和亚化学计量的五氧化三钛（β-Ti3O5）组成。Ti3O5作为超薄的外层包裹着锐钛矿NPs，或者生长在锐钛矿表面，形成随机分布的“纳米岛”，与Sc3+离子紧密相连。在空气下加热到800℃，Sc3+从锐钛矿晶格中分离出来，形成富sc的氧化物（通常为Sc4Ti3O12）。同时，检测到Ti4+含量的增加以Ti3+含量的减少为代价。x射线光电子能谱（XPS）研究了这些元素的表面组成、氧化态和电子构型，结果表明，相对于Sc和Ti的总和，Sc含量为4.6%，接近名义成分的4%。XPS和EELS对4SDT的O/Ti值分别为2.3±0.1和2.2±0.2。

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来源期刊

Materials Characterization 工程技术-材料科学：表征与测试

CiteScore

7.60

自引率

8.50%

发文量

746

审稿时长

36 days

期刊介绍： Materials Characterization features original articles and state-of-the-art reviews on theoretical and practical aspects of the structure and behaviour of materials. The Journal focuses on all characterization techniques, including all forms of microscopy (light, electron, acoustic, etc.,) and analysis (especially microanalysis and surface analytical techniques). Developments in both this wide range of techniques and their application to the quantification of the microstructure of materials are essential facets of the Journal. The Journal provides the Materials Scientist/Engineer with up-to-date information on many types of materials with an underlying theme of explaining the behavior of materials using novel approaches. Materials covered by the journal include: Metals & Alloys Ceramics Nanomaterials Biomedical materials Optical materials Composites Natural Materials.