Direct Observation of Carbonate Formation in Partly Hydrated Tricalcium Silicate by Dynamic Nuclear Polarization Enhanced NMR Spectroscopy

Direct Observation of Carbonate Formation in Partly Hydrated Tricalcium Silicate by Dynamic Nuclear Polarization Enhanced NMR Spectroscopy
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通过动态核极化增强核磁共振波谱直接观察部分水合硅酸三钙中碳酸盐的形成

DOI:
10.1021/acs.jpcc.0c10382
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发表时间:
2021
影响因子:
3.7
通讯作者:
G. Buntkowsky
G. Buntkowsky
中科院分区:
化学3区
文献类型:
--
作者:
V. Klimavicius;H. Hilbig;T. Gutmann;G. Buntkowsky

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采用固态核磁共振结合动态核极化(DNP NMR)技术研究了硅酸三钙(Ca3SiO5,简称C3S)样品的水化过程。所研究的C3S样品经历了早期水化(1 ~ 30 h)和缓慢老化(9年)过程。部分水化C3S样品的29Si MAS和1h→29Si CP MAS核磁共振谱中q3和q4谱线的出现表明无定形二氧化硅的形成与碳酸化相对应,并通过互补的FTIR数据证实了这一点。所研究样品的显著DNP信号增强使我们能够利用1h→29Si CP MAS FSLG hetor技术进一步详细研究C3S碳化过程。最后,DNP增强了1h→13C CP MAS和1h→13C CP MAS FSLG hetor技术,可以直接观察部分水合C3S样品中碳酸盐组分的形成。
Solid-state NMR combined with dynamic nuclear polarization (DNP NMR) is used to study hydration processes in tricalcium silicate (Ca3SiO5, abbreviated as C3S) samples. The studied C3S samples have experienced early stage hydration (1–30 h) and slow aging (9 years) processes. The appearance of Q3and Q4lines in the29Si MAS and1H →29Si CP MAS NMR spectra obtained for partly hydrated C3S samples indicated the formation of amorphous silica which corresponds to their carbonation, which was corroborated by complementary FTIR data. Significant DNP signal enhancements obtained for the studied samples allowed to further investigate the C3S carbonation process in detail employing the1H →29Si CP MAS FSLG HETCOR technique. Finally, DNP enhanced1H →13C CP MAS and1H →13C CP MAS FSLG HETCOR techniques enabled to directly observe the formation of carbonate moieties in partly hydrated C3S samples.
氢键引起 CO3 单元变形和无定形碳酸钙的动力学稳定性:2D (13)C NMR 光谱的结果。
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