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首页> 外文期刊>Journal of Sol-Gel Science and Technology >Spectroscopic monitoring of sol-gel syntheses of heterometallic ceramics
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Spectroscopic monitoring of sol-gel syntheses of heterometallic ceramics

机译：光谱监测异金属陶瓷的溶胶-凝胶合成

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Multinuclear NMR spectroscopy and mass spectrometry have been used to monitor the sol-gelsyntheses of heterometallic ceramics. Hydrolytic and non-hydrolytic sol-gelprocedures have beenused for the synthesis of NASICON,Na_3Zr_2Si_2PO_(12).In the hydrolytic process the precursors were slowly gelated under exposre to atmospheric moisture. 1D and 2D NMR measureemnt allowed to follow the advancement of the reaction and determine the degre of polymerization. In the non-hydrolytic process the spectroscopic analysis allowed to establish the reaction mechanism and to optimize the synthetic conditions. After thermaltreatments a very high quality NASICON phase has been obtained as shown by XRD. Three different procedures have been used with the aim of preparing thin films of betaSl_2TiO_5 by hydrolysis of alkoxides of the two metals in acidic condition with or without 2,4-pentanedione (acac) as a chelating agent. Both NMR and MS indicated as the best synthess the one carried out without acac. XRD patterns of the films obtained confirmed the results of the spectroscopic analysis.
机译：多核NMR光谱法和质谱法已经用于监测异金属陶瓷的溶胶-凝胶合成。水解和非水解溶胶-凝胶过程已用于合成NASICON，Na_3Zr_2Si_2PO_（12）。在水解过程中，前体在暴露于大气水分的条件下缓慢凝胶化。 1D和2D NMR测量可以跟踪反应的进行并确定聚合度。在非水解过程中，光谱分析可以建立反应机理并优化合成条件。热处理后，如XRD所示，已获得了非常高质量的NASICON相。已经使用了三种不同的程序，目的是通过在酸性条件下，在有或没有2,4-戊二酮（acac）作为螯合剂的情况下，通过水解两种金属的醇盐来制备βSl_2TiO_5薄膜。 NMR和MS均表明，最好的合成方法是不使用acac进行的合成。获得的膜的XRD图谱证实了光谱分析的结果。

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