Eu-doped LDH合成、有机插层及其发光性质研究
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摘要
层状双氢氧化物(layered double hydroxide, LDH)因其特有的层间通道结构引起科研界的关注。目前关于LDH的研究主要集中在层间离子交换、有机插层、剥离／再配列等,而关于其发光特性方面的研究仍然不足。尽管有个别研究涉及层间插入有机发光层,或制备具有发光性质的稀土层状化合物,但从廉价的原料及简单的工艺角度考虑,在通常廉价的LDH层板上引入发光离子的研究还是值得探索,并具有一定的意义。
为此,本文采用共沉淀法合成了一系列M2+/M3+摩尔比不同的三元Mg-Al-Eu LDH (Layered Double Hydroxide)和Zn-Al-Eu LDH,并对这些产物的结构、组成和发光性质进行了研究；研究了退火温度对Mg-Al-Eu LDH和Zn-Al-Eu LDH的结构和发光的影响；在此基础上进一步研究了Mg-Al-Eu LDH和Zn-Al-Eu LDH的荧光对苯丙氨酸的敏感性。通过这些研究获得了一些具有创新意义的结果：
1.首次在层板上掺入Eu而得到具有发光性质的LDH结构的化合物。研究发现,LDH结构和结晶性与M2+/M3+摩尔比(M3+:A13++Eu3+; M2+:Mg2+, Zn2+)有着依赖关系。
2.关于Mg-Al-Eu LDH和Zn-Al-Eu LDH的退火研究发现,随着退火温度的升高,LDH的结构和荧光发生明显的变化。Mg-Al-Eu LDH的层板结构在400℃被破坏,而Zn-Al-EuLDH的层板在200℃时开始被破坏。这表明Mg-Al-Eu LDH的结构比Zn-Al-Eu LDH的结构更稳定,而且在LDH和其所有的退火产物都有利于Eu3+的发光。
3.关于Mg-Al-Eu LDH和Zn-Al-Eu LDH的荧光对苯丙氨酸(Phen)的敏感性研究发现,Phen对Mg-Al-Eu LDH及Zn-Al-Eu LDH的荧光具有明显的淬灭作用。这种淬灭作用可能主要源于LDH与Phen之间的相互作用。利用Phen对LDH荧光淬灭这点性质,可使Mg-Al-Eu LDH及Zn-Al-Eu LDH作为一种潜在的生物荧光探针材料,来探测蛋白质或DNA的结构变换。这种具有层间通道结构的生物荧光探针材料比其它结构的体材料具有更大的表面积,比纳米和有机生物荧光材料具有更高的热稳定性,并比有有机生物荧光材料具有更小的毒性,对人体更健康。
Layered double hydroxides (LDHs) have been attracted because of its special interlayer tunnel structure. At present, the study on LDHs is mainly focused on ion-exchanges, organic intercalation and exfoliation/self-assembly etc., while the study on the luminescence of LDHs is quite insufficient. Although some attempts at intercalation of rare earth ions complex into the interlayer of LDHs and preparation of rare earth layered compounds with emission property, it is worthwhile to investigate the incorporation of luminescent centers into the layer in views of cheap raw and simple processing.
Therefore, a serials of ternary LDHs (Mg-Al-Eu and Zn-Al-Eu LDHs) with different M2+/(M3+) molar ratios have been synthesized by co-precipitate method (M3+:Al3++Eu3+; M2+:Mg2+, Zn2+) in the paper, and their chemical composition, structure, and photoluminescent property have been investigated. In addition, the study on the effects of annealing temperature on the structure and photoluminescent property has been carried out. Furthermore, the fluorescence of Mg-Al-Eu and Zn-Al-Eu LDHs sensitivity to Phenylalanine has also been researched. From these work, some original results were found as following:
1. Eu+-doped layered double hydroxides with photoluminescence were synthesized at the first time. It was found that the structure and crystallinity of LDHs obviously depended on the M+/M+molar ratios.
2. The study on the effects of annealing temperature on the Mg-Al-Eu LDH and Zn-Al-Eu LDH showed that the structure and fluorescence of LDHs changed with the increase of annealing temperature. The layered structure of the Mg-Al-Eu LDH collapsed as annealing temperature increased to 400℃, but the structure of the Zn-Al-Eu LDH was broken up at 200℃. This indicated that thermal stability of the Mg-Al-Eu LDH was higher than that of the Zn-Al-Eu LDH. It was also confirmed that the LDHs and their annealed products were favorable for the Eu3+ emissions.
3. The research on the fluorescence of Mg-Al-Eu and Zn-Al-Eu LDHs sensitive to phenylalanine indicated that the fluorescence attributed to those LDHs are almost quenched by the phenylalanine, which is an important property to be used in biological technique probe the changes of DNA or Proteins. This special interlayer tunnel structural material may be a promising candidate for fluorescent material applied in biological probe, which would be possessed of larger surface area than other structural bulk materials, higher thermal stability and less toxicity compared with those of organic materials, and healthier to human beings.
为此,本文采用共沉淀法合成了一系列M2+/M3+摩尔比不同的三元Mg-Al-Eu LDH (Layered Double Hydroxide)和Zn-Al-Eu LDH,并对这些产物的结构、组成和发光性质进行了研究；研究了退火温度对Mg-Al-Eu LDH和Zn-Al-Eu LDH的结构和发光的影响；在此基础上进一步研究了Mg-Al-Eu LDH和Zn-Al-Eu LDH的荧光对苯丙氨酸的敏感性。通过这些研究获得了一些具有创新意义的结果：
1.首次在层板上掺入Eu而得到具有发光性质的LDH结构的化合物。研究发现,LDH结构和结晶性与M2+/M3+摩尔比(M3+:A13++Eu3+; M2+:Mg2+, Zn2+)有着依赖关系。
2.关于Mg-Al-Eu LDH和Zn-Al-Eu LDH的退火研究发现,随着退火温度的升高,LDH的结构和荧光发生明显的变化。Mg-Al-Eu LDH的层板结构在400℃被破坏,而Zn-Al-EuLDH的层板在200℃时开始被破坏。这表明Mg-Al-Eu LDH的结构比Zn-Al-Eu LDH的结构更稳定,而且在LDH和其所有的退火产物都有利于Eu3+的发光。
3.关于Mg-Al-Eu LDH和Zn-Al-Eu LDH的荧光对苯丙氨酸(Phen)的敏感性研究发现,Phen对Mg-Al-Eu LDH及Zn-Al-Eu LDH的荧光具有明显的淬灭作用。这种淬灭作用可能主要源于LDH与Phen之间的相互作用。利用Phen对LDH荧光淬灭这点性质,可使Mg-Al-Eu LDH及Zn-Al-Eu LDH作为一种潜在的生物荧光探针材料,来探测蛋白质或DNA的结构变换。这种具有层间通道结构的生物荧光探针材料比其它结构的体材料具有更大的表面积,比纳米和有机生物荧光材料具有更高的热稳定性,并比有有机生物荧光材料具有更小的毒性,对人体更健康。
Layered double hydroxides (LDHs) have been attracted because of its special interlayer tunnel structure. At present, the study on LDHs is mainly focused on ion-exchanges, organic intercalation and exfoliation/self-assembly etc., while the study on the luminescence of LDHs is quite insufficient. Although some attempts at intercalation of rare earth ions complex into the interlayer of LDHs and preparation of rare earth layered compounds with emission property, it is worthwhile to investigate the incorporation of luminescent centers into the layer in views of cheap raw and simple processing.
Therefore, a serials of ternary LDHs (Mg-Al-Eu and Zn-Al-Eu LDHs) with different M2+/(M3+) molar ratios have been synthesized by co-precipitate method (M3+:Al3++Eu3+; M2+:Mg2+, Zn2+) in the paper, and their chemical composition, structure, and photoluminescent property have been investigated. In addition, the study on the effects of annealing temperature on the structure and photoluminescent property has been carried out. Furthermore, the fluorescence of Mg-Al-Eu and Zn-Al-Eu LDHs sensitivity to Phenylalanine has also been researched. From these work, some original results were found as following:
1. Eu+-doped layered double hydroxides with photoluminescence were synthesized at the first time. It was found that the structure and crystallinity of LDHs obviously depended on the M+/M+molar ratios.
2. The study on the effects of annealing temperature on the Mg-Al-Eu LDH and Zn-Al-Eu LDH showed that the structure and fluorescence of LDHs changed with the increase of annealing temperature. The layered structure of the Mg-Al-Eu LDH collapsed as annealing temperature increased to 400℃, but the structure of the Zn-Al-Eu LDH was broken up at 200℃. This indicated that thermal stability of the Mg-Al-Eu LDH was higher than that of the Zn-Al-Eu LDH. It was also confirmed that the LDHs and their annealed products were favorable for the Eu3+ emissions.
3. The research on the fluorescence of Mg-Al-Eu and Zn-Al-Eu LDHs sensitive to phenylalanine indicated that the fluorescence attributed to those LDHs are almost quenched by the phenylalanine, which is an important property to be used in biological technique probe the changes of DNA or Proteins. This special interlayer tunnel structural material may be a promising candidate for fluorescent material applied in biological probe, which would be possessed of larger surface area than other structural bulk materials, higher thermal stability and less toxicity compared with those of organic materials, and healthier to human beings.
引文
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