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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >ZnO Nanoparticle Formation from the Molecular Precursor MeZnOtBu(4) by Ozone Treatment in Ionic Liquids: in-situ Vibrational Spectroscopy in an Ultrahigh Vacuum Environment
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ZnO Nanoparticle Formation from the Molecular Precursor MeZnOtBu(4) by Ozone Treatment in Ionic Liquids: in-situ Vibrational Spectroscopy in an Ultrahigh Vacuum Environment

机译：离子液体中臭氧处理分子前驱体MeZnOtBu（4）形成ZnO纳米颗粒：超高真空环境下的原位振动光谱

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摘要

As reported previously, novel ZnO nanostructures can be grown by oxidation of MeZnOtBu(4) building blocks with O-3 in ionic liquids (ILs). In this study, we have explored the role of the IL during ZnO formation by in-situ infrared reflection absorption spectroscopy (IRAS) in ultrahigh vacuum (UHV). MeZnOtBu(4) and C(2)C(1)ImOTf were (co-)deposited as thin films by physical vapor deposition (PVD) onto Au(111), separately or simultaneously. The IR spectrum of MeZnOtBu(4) was analyzed between 300 and 4000 cm(-1) based on calculated spectra from density-functional theory (DFT). Spectral changes in the IL-related bands during the thermal treatment of MeZnOtBu(4) in C(2)C(1)ImOTf indicate the loss of the precursor ligands and the interaction of the IL with the growing ZnO aggregates. The films were treated with ozone (10(-6) mbar) in UHV and the spectral changes were monitored in-situ by IRAS. Slow ozonolysis of C(2)C(1)ImOTf is observed. Spectroscopically we identify the primary ozonide formed by addition of O-3 to C(2)C(1)Im(+) and suggest a reaction mechanism, which leads to a biuret derivative. Upon ozone treatment of mixed MeZnOtBu(4)/C(2)C(1)ImOTf films, ZnO aggregates are formed at the IL/vacuum interface. Ozonolysis of C(2)C(1)ImOTf is suppressed. Upon annealing to 320 K, further ZnO aggregates are formed, leading to enclosure of C(2)C(1)ImOTf in the ZnO film. At 380 K the IL is released from the mixed film. The pure C(2)C(1)ImOTf desorbs at 420 K, leaving behind the ZnO phase.
机译：如前所述，在离子液体 （IL） 中，通过用 O-3 氧化 [MeZnOtBu]（4） 砌块，可以生长出新型 ZnO 纳米结构。在这项研究中，我们通过超高真空（UHV）中的原位红外反射吸收光谱（IRAS）探讨了IL在ZnO形成过程中的作用。[MeZnOtBu]（4）和[C（2）C（1）Im][OTf]分别或同时通过物理气相沉积（PVD）沉积为薄膜到Au（111）上。根据密度泛函理论（DFT）计算的光谱，分析了[MeZnOtBu]（4）在300-4000 cm（-1）之间的红外光谱。在[C（2）C（1）Im][OTf]中对[MeZnOtBu]（4）进行热处理过程中IL相关谱带的光谱变化表明前体配体的丢失以及IL与生长的ZnO聚集体的相互作用。在UHV中用臭氧（10（-6）mbar）处理薄膜，并通过IRAS原位监测光谱变化。观察到[C（2）C（1）Im][OTf]的缓慢臭氧分解。在光谱学上，我们确定了由O-3添加到[C（2）C（1）Im]（+）中形成的初级臭氧化物，并提出了一种反应机理，该机理导致缩二脲衍生物。对混合[MeZnOtBu]（4）/[C（2）C（1）Im][OTf]薄膜进行臭氧处理后，在IL/真空界面处形成ZnO聚集体。[C（2）C（1）Im][OTf]的卵解被抑制。在退火至320 K时，形成进一步的ZnO聚集体，导致[C（2）C（1）Im][OTf]在ZnO薄膜中包裹。在 380 K 时，IL 从混合薄膜中释放出来。纯 [C（2）C（1）Im][OTf] 在 420 K 时解吸，留下 ZnO 相。

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