CAJ | 학술논문

利用程序控温的水热合成法得到了两种含有2，2′-bipy及[M oO3]簇骼的化合物：[（2，2′-bipy ）2（MoO3）3]n（Ⅰ）和[（2，2′-bipy）（MoO3）]n（Ⅱ）。为了阐明这两个化合物结构与谱学的关系，通过XRD、FT-IR、热微扰2D-IR相关光谱、TG分析、SEM、高温红外分析、UV-Vis DRS光谱和固体荧光光谱研究手段进行研究，进而探讨结构与性能的关系。其XRD说明了化合物Ⅰ和Ⅱ是纯物相；FT IR的特征振动频率和热微扰2D-IR相关光谱的响应峰与化合物Ⅰ和Ⅱ的结构解析相一致，2D-IR的同步和异步相关光谱图还确定了化合物Ⅰ和Ⅱ的钼氧簇骼振动强度随升温变化的先后顺序与高温红外解析相一致；通过 TG分析和高温红外分析研究化合物Ⅰ和Ⅱ的热稳定性；化合物Ⅰ和Ⅱ的UV-Vis DRS光谱显示在225～350 nm有宽的紫外吸收谱带；化合物Ⅰ和Ⅱ的固体荧光光谱分别在277和295 nm的激发下得到的最强发射峰值分别为460和480 nm。本文阐明了化合物Ⅰ和Ⅱ的配位情况，揭示了价电子在分子中相应能级间跃迁的内在规律；还验证了弱相互作用力在配合物的结构框架中不但起稳定作用，而且在耐热性扮演重要的角色。
이용정서공온적수열합성법득도료량충함유2，2′-bipy급[M oO3]족격적화합물：[（2，2′-bipy ）2（MoO3）3]n（Ⅰ）화[（2，2′-bipy）（MoO3）]n（Ⅱ）。위료천명저량개화합물결구여보학적관계，통과XRD、FT-IR、열미우2D-IR상관광보、TG분석、SEM、고온홍외분석、UV-Vis DRS광보화고체형광광보연구수단진행연구，진이탐토결구여성능적관계。기XRD설명료화합물Ⅰ화Ⅱ시순물상；FT IR적특정진동빈솔화열미우2D-IR상관광보적향응봉여화합물Ⅰ화Ⅱ적결구해석상일치，2D-IR적동보화이보상관광보도환학정료화합물Ⅰ화Ⅱ적목양족격진동강도수승온변화적선후순서여고온홍외해석상일치；통과 TG분석화고온홍외분석연구화합물Ⅰ화Ⅱ적열은정성；화합물Ⅰ화Ⅱ적UV-Vis DRS광보현시재225～350 nm유관적자외흡수보대；화합물Ⅰ화Ⅱ적고체형광광보분별재277화295 nm적격발하득도적최강발사봉치분별위460화480 nm。본문천명료화합물Ⅰ화Ⅱ적배위정황，게시료개전자재분자중상응능급간약천적내재규률；환험증료약상호작용력재배합물적결구광가중불단기은정작용，이차재내열성분연중요적각색。
Two compounds of molybdate with 2 ,2′-bipy and [MoO3 ]:[(2 ,2′-bipy )2 (MoO3 )3 ]n (Ⅰ ) and [(2 ,2′-bipy ) (MoO3 )]n (Ⅱ ) were successfully synthesized by hydrothermal synthesis method with programmable temperature control .In order to clarify the relationship between the structure and spectroscopy of these two compounds ,both of them were characterized by means of X-ray powder diffraction (XRD) ,Fourier transform infrared spectra(FTIR) ,thermal perturbation 2D-IR correla-tion spectrum (2D-IR COS) ,thermogravimetric analysis(TGA) ,scanning electron microscopy(SEM) ,High temperature infra-red analysis ,UV-Vis DRS adsorption spectra and solid fluorescence spectrum to investigate the relationship between structure and properties of the title compounds .The powder XRD patterns of the complexes are well matched with the simulation based on single-crystal analysis ,which indicate that compound Ⅰ and Ⅱ are in a pure phase .The characteristics of vibration frequency of FTIR and thermal perturbation relative spectral response of 2D-IR peak is consistent with the compound Ⅰ and Ⅱ structure a-nalysis .The synchronous and asynchronous correlation 2D-IR spectra of compounds also identified the compounds Ⅰ and Ⅱ mo-lybdenum-oxygen cluster skeletons sequencing of vibration intensity change with temperature consistent with the high tempera-ture infrared analysis .Through the TGA and high temperature infrared analysis it was found that the decomposition temperature was more than 300 ℃ and maximum weight losses rates above 800 ℃ ,which suggest that they have good thermal stability .Ac-cording to the UV-Vis DRS spectrum of the compound Ⅰ and Ⅱ there exists a wide ultraviolet absorption band in a range of 225 to 350 nm .The compound Ⅰand Ⅱ steady-state fluorescence spectrum under the excitation of 277 and 295 nm respectively re-vealed compound Ⅰ and Ⅱ have the strongest emission peak at 460 and 480 nm respectively .This paper illustrates the coordina-tion situation of these two compounds ,and reveals the inherent law of valence electrons in molecule energy level transition .In the meantime it was verified that the weak interaction not only plays a role of stability in the frame of the structure of the comple-xes ,but also plays an important role in heat resistance .