Crystallization Pathway of Size-Controlled SnO2 Nanoparticles Synthesized via a Nonaqueous Sol–Gel Route,Crystal Growth & Design

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Crystallization Pathway of Size-Controlled SnO2 Nanoparticles Synthesized via a Nonaqueous Sol–Gel Route
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2020-01-22 , DOI: 10.1021/acs.cgd.9b01428
Alex Lemarchand ₁ , Fabien Rémondière ₁ , Jenny Jouin ₁ , Philippe Thomas ₁ , Olivier Masson ₁

Affiliation

This paper deals with the crystallization pathway of tin dioxide nanoparticles of a few nanometers synthesized via a nonaqueous sol–gel route based on the etherolysis of a tin tetrachloride (SnCl₄) precursor. Two different ethers were used as oxygen donors: diisopropyl ether (ⁱPr₂O) and dibenzyl ether (Bn₂O). The solvothermal treatments of SnCl₄ in ⁱPr₂O at different temperatures and reaction times revealed in the early stages of the reaction the formation of an organic polymeric phase in which crystalline nanoparticles are embedded. In the case of the SnCl₄–Bn₂O system, the formation of a brownish polymer containing crystalline oxidic nanoparticles and the production of water were evidenced. With both ethers, an unexpected intermediate disordered nanocrystalline phase is formed, which progressively transforms into rutile-type SnO₂ nanoparticles. The formation of the polymeric phase, which is suspected to act as a trap for the nanoparticles, freezes the intermediate phase, limits the particle growth, and delays the restructuration into the rutile-type structure. The degradation of the polymer phase in the case of ⁱPr₂O and/or the water action in the case of Bn₂O are finally able to destabilize the nanoparticle–polymer assembly and to induce the restructuration of the nanoparticles.

中文翻译：

通过非水溶胶-凝胶路线合成的尺寸受控的SnO ₂纳米颗粒的结晶途径

本文研究了基于四氯化锡（SnCl ₄）前体的醚解作用，通过非水溶胶-凝胶途径合成的几纳米二氧化锡纳米颗粒的结晶途径。两种不同的醚用作供氧体：二异丙醚（ⁱ Pr ₂ O）和二苄基醚（Bn ₂ O）。在不同的温度和反应时间下，对ⁱ Pr ₂ O中的SnCl ₄进行溶剂热处理表明，在反应的早期阶段，形成了嵌入结晶纳米颗粒的有机聚合物相。对于SnCl ₄ -Bn ₂在O体系中，证实了包含结晶性氧化纳米颗粒的褐色聚合物的形成和水的产生。使用这两种醚，会形成意外的中间无序纳米晶相，该相逐渐转变为金红石型SnO ₂纳米颗粒。疑似充当纳米颗粒陷阱的聚合物相的形成，冻结了中间相，限制了颗粒的生长，并延迟了重组为金红石型结构的过程。在ⁱ Pr ₂ O的情况下，聚合物相的降解和/或在Bn ₂ O的情况下，水的作用最终能够破坏纳米颗粒-聚合物的组装并诱导纳米颗粒的重组。

更新日期：2020-01-23

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