微孔复合材料的制备、表征以及性能研究
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摘要
随着科学技术的不断进步，单一组分材料所具有的性能已经无法满足人们日益增长的需求。复合材料具有单一组分所不具备的多种新奇性质和优越性能。因此，在过去的20年间，关于复合材料的研究飞速发展，越来越多的新型复合材料不断地被研制开发，而它们的多种特异性能也展现出了良好的应用前景。在无机复合材料中，微孔分子筛无疑是最为理想的主体载体材料之一。其特殊的孔道结构以及良好的机械与热稳定性，使其受到科研工作者的青睐。因此开发以分子筛为主体的复合材料无论对于科学研究还是实际应用都有重要的意义。
发光材料广泛应用于人民生活的各个领域，从日常生活的灯光照明，荧光管，投影电视到工业用的阴极射线管、可调变激光、发光二极管以及医用的X射线增感屏都包含了发光材料。本论文首先以微孔分子筛为主体合成了一系列具有良好荧光性能的复合发光材料，这些复合材料以限制于微孔分子筛孔道内的碳基纳米粒子为发光中心，显示出了良好的热稳定性以及发光波长调变性能。通过改变实验条件，其发光波长可以从420nm调变到550nm。其次，采用水相合成法分别以已合成的复合发光材料和生物质材料—两种树木的落叶为原料合成三种水溶性荧光碳基纳米粒子，并详细研究了三种样品的荧光性质及其在生物活性和细胞荧光标记方面的应用性能。结果显示，三种发光材料对于细胞显示为无毒性，并具有良好的细胞荧光标记性能，是生物医学领域潜在的应用材料。最后在微孔分子筛孔道内以单核一价锌为基础合成出了两种II-V半导体材料氮化锌与磷化锌。其中氮化锌材料表现出良好的室温可见光区的荧光性质；而磷化锌材料作为蒸发源，通过真空气相沉积方法，可以一次性在同一基底上得到多种氮化锌的低维纳米级结构。
With the continuous progress of science and technology, the performance ofthe single-component materials has been unable to meet the growing demand forpractical application. Composite materials have displayed a variety of novelproperties and superior performance which are not available in the single-componentmaterials. Therefore, the research on the composite materials underwent a rapiddevelopment in the past two decades. More and more new composite materials havebeen synthesized, and their specific properties have shown good prospects forapplications. Among the inorganic composite materials, microporous molecularsieve is undoubtedly one of the most ideal host materials. Its special pore structureand good mechanical and thermal stability make it favored by scientific researchers.Molecular sieve-based composite materials have great applications in a variety range.For example, in the field of gas storage and separation, drug delivery, industrialcatalysis and so on, they have exhibited good performance and promoted the relatedresearch. Therefore the exploiture of molecular sieve-based composite materials hasa great significance both for the scientific research and the practical application.
In this paper, firstly, microporous molecular sieve was chosen as the hostmaterials to synthesize a series fluorescent composite material with goodphotoluminescence performance. Secondly, on the basis of previous work, we usethe synthesized molecular sieve-based composite materials and biomaterial defoliation as the raw material to prepare two kinds of water-soluble carbogenicnanoparticles. These nanoparticles are almost nontoxic for human cells and idealcellular imaging agents. Finally, according to the principles of CVD, a set of vacuumchemical vapor reaction system was designed, which was used to prepare zincphosphide and zinc nitride semiconductor nanomaterials in the host microporousmolecular sieve. This thesis is divided into four parts.
In chapter one, we introduced the research background of this thesis andsummarized the development process and status of host-guest composite materials.Then emphasis was given to the prospect of porous material-based luminescentmaterial on the development of its synthesis and property, as well as the practicalapplication and potential barriers of luminescent material in the biomedical field.After that, we focused on the situation of low-dimensional materials synthesized inthe condition of vacuum. Finally, the significance and achievement was brieflydescribed.
Well-defined synthesis conditions allow microporous molecular sieve materialsto be highly transparent in the UV and visible regions. In chapter two, CNP-loadedmagnesium-aluminophosphate solid phosphors have been prepared through thermaldecomposition of the occluded template or loaded organic molecules. It is revealedthat the carbogenic species in the phosphors is responsible for the observedphotoluminescence, and the emission wavelength depends on the carbon content inthe materials. XPS and ESR spectroscopies demonstrate that the PL property arisesfrom defects which render electron localization in the CNPs possible. Uponirradiation with UV light, the surface states with the localized electrons in the CNPsare excited, whereas the radiative relaxation of the excited surface states releasesenergy, emitting visible light. The emission intensity is also correlated with thecarbon content in the phosphor materials. At a lower carbon content, the emissionintensity increases with the content, whereas at a higher carbon content, the emissionintensity is inversely proportional to the content because of the competition betweenconcentration contribution and quenching of the luminescent centers in the phosphor. These phosphor materials possess high thermal stability and tunable emissionwavelength. Through varying the thermal treatment condition, the emissionwavelength can be tuned from420to550nm.
In chapter three, we use an aqueous route to synthesize three samples of watersoluble carbogenic nanoparticles. The solid phosphors in the previous chapter and twokinds of biomaterial defoliation were used as the raw materials. Their performance inphotoluminescence, cytotoxicity and cellular imaging was investigated in detail. Theresults showed that, the defoliation-derived carbogenic nanoparticles exhibited thetypical excitation-dependent emission, which may reflect not only effects fromparticles of different sizes in the sample but also a distribution of different emissivesites on the carbogenic nanoparticles. On the other hand, the solid phosphor-derivedsample displayed the excitation-independent emission, implying its relatively simplechemical environment. All the three samples have good photostability and are stablein a solution at high ionic strength of5M. NaCl. In the HeLa cell survival test, all thecarbogenic nanoparticles exhibited low cytotoxicity. Especially in the highconcentration, the performance of all the samples were superior to that of thetraditional quantum dots, which render them better prospects for the biologicallabeling. In the following cell imaging to human embryonic kidney cells, all thesamples enter into cells without any further functionalization, and exhibit obviousphotoluminescence signal. In particular, the solid phosphor-derived sample penetratedinto the karyon without the modification with specific transferrable protein, and usingits fluorescence property, it is possible track the carbogenic nanoparticles. All thebiological results indicates that the three samples of carbogenic nanoparticles is ableto used as fluorescent probe molecules in cellular imaging and bio-detection.Moreover, there is no distinct difference in the photoluminescence property,cytotoxicity, and cell labeling results of these two kinds of defoliation-derivedcarbogenic nanoparticles, suggesting that the aqueous route we used for thepreparation of water soluble carbogenic nanoparticles is generally universal, and maybe extended to various defoliations.
In chapter four, the elemental zinc was introduced into the cages of microporousmagnesium-aluminophosphate and silicoaluminophosphate molecular sieve,respectively, using the designed vacuum chemical vapor reaction system. Elementalzinc reacted with the proton in the framework and the univalent zinc was generated.For the magnesium-aluminophosphate system, the formation of univalent zinc leadedthe dephosphorization on the framework. The removed phosphorus reacted withpartial univalent zinc, and generated zinc phosphide. We use the zincphosphide-loaded composite material as the evaporation source to synthesize a seriesof low-dimensional nanostructures of zinc phosphide on one substrate, includingnanoparticles, nanowires, and dense zinc phosphide films. The results show that thegrowth of zinc phosphide nanostructures follows the vapor-solid mechanism. On theother hand, for the silicoaluminophosphate system, ammonia molecules areintroduced into the univalent zinc-contained molecular sieve in sequence. At roomtemperature, the univalent zinc reacted with ammonia, resulting in zinc nitride in themicroporous, and the reaction is exothermic. The resulted zinc nitride-loadedmicroporous composite material displayed a certain room temperaturephotoluminescence. Since the high temperature or complicated equipment is alwaysneeded in its preparation, zinc nitride directly synthesized from ammonia at roomtemperature have not been achieved yet prior to our work.
发光材料广泛应用于人民生活的各个领域，从日常生活的灯光照明，荧光管，投影电视到工业用的阴极射线管、可调变激光、发光二极管以及医用的X射线增感屏都包含了发光材料。本论文首先以微孔分子筛为主体合成了一系列具有良好荧光性能的复合发光材料，这些复合材料以限制于微孔分子筛孔道内的碳基纳米粒子为发光中心，显示出了良好的热稳定性以及发光波长调变性能。通过改变实验条件，其发光波长可以从420nm调变到550nm。其次，采用水相合成法分别以已合成的复合发光材料和生物质材料—两种树木的落叶为原料合成三种水溶性荧光碳基纳米粒子，并详细研究了三种样品的荧光性质及其在生物活性和细胞荧光标记方面的应用性能。结果显示，三种发光材料对于细胞显示为无毒性，并具有良好的细胞荧光标记性能，是生物医学领域潜在的应用材料。最后在微孔分子筛孔道内以单核一价锌为基础合成出了两种II-V半导体材料氮化锌与磷化锌。其中氮化锌材料表现出良好的室温可见光区的荧光性质；而磷化锌材料作为蒸发源，通过真空气相沉积方法，可以一次性在同一基底上得到多种氮化锌的低维纳米级结构。
With the continuous progress of science and technology, the performance ofthe single-component materials has been unable to meet the growing demand forpractical application. Composite materials have displayed a variety of novelproperties and superior performance which are not available in the single-componentmaterials. Therefore, the research on the composite materials underwent a rapiddevelopment in the past two decades. More and more new composite materials havebeen synthesized, and their specific properties have shown good prospects forapplications. Among the inorganic composite materials, microporous molecularsieve is undoubtedly one of the most ideal host materials. Its special pore structureand good mechanical and thermal stability make it favored by scientific researchers.Molecular sieve-based composite materials have great applications in a variety range.For example, in the field of gas storage and separation, drug delivery, industrialcatalysis and so on, they have exhibited good performance and promoted the relatedresearch. Therefore the exploiture of molecular sieve-based composite materials hasa great significance both for the scientific research and the practical application.
In this paper, firstly, microporous molecular sieve was chosen as the hostmaterials to synthesize a series fluorescent composite material with goodphotoluminescence performance. Secondly, on the basis of previous work, we usethe synthesized molecular sieve-based composite materials and biomaterial defoliation as the raw material to prepare two kinds of water-soluble carbogenicnanoparticles. These nanoparticles are almost nontoxic for human cells and idealcellular imaging agents. Finally, according to the principles of CVD, a set of vacuumchemical vapor reaction system was designed, which was used to prepare zincphosphide and zinc nitride semiconductor nanomaterials in the host microporousmolecular sieve. This thesis is divided into four parts.
In chapter one, we introduced the research background of this thesis andsummarized the development process and status of host-guest composite materials.Then emphasis was given to the prospect of porous material-based luminescentmaterial on the development of its synthesis and property, as well as the practicalapplication and potential barriers of luminescent material in the biomedical field.After that, we focused on the situation of low-dimensional materials synthesized inthe condition of vacuum. Finally, the significance and achievement was brieflydescribed.
Well-defined synthesis conditions allow microporous molecular sieve materialsto be highly transparent in the UV and visible regions. In chapter two, CNP-loadedmagnesium-aluminophosphate solid phosphors have been prepared through thermaldecomposition of the occluded template or loaded organic molecules. It is revealedthat the carbogenic species in the phosphors is responsible for the observedphotoluminescence, and the emission wavelength depends on the carbon content inthe materials. XPS and ESR spectroscopies demonstrate that the PL property arisesfrom defects which render electron localization in the CNPs possible. Uponirradiation with UV light, the surface states with the localized electrons in the CNPsare excited, whereas the radiative relaxation of the excited surface states releasesenergy, emitting visible light. The emission intensity is also correlated with thecarbon content in the phosphor materials. At a lower carbon content, the emissionintensity increases with the content, whereas at a higher carbon content, the emissionintensity is inversely proportional to the content because of the competition betweenconcentration contribution and quenching of the luminescent centers in the phosphor. These phosphor materials possess high thermal stability and tunable emissionwavelength. Through varying the thermal treatment condition, the emissionwavelength can be tuned from420to550nm.
In chapter three, we use an aqueous route to synthesize three samples of watersoluble carbogenic nanoparticles. The solid phosphors in the previous chapter and twokinds of biomaterial defoliation were used as the raw materials. Their performance inphotoluminescence, cytotoxicity and cellular imaging was investigated in detail. Theresults showed that, the defoliation-derived carbogenic nanoparticles exhibited thetypical excitation-dependent emission, which may reflect not only effects fromparticles of different sizes in the sample but also a distribution of different emissivesites on the carbogenic nanoparticles. On the other hand, the solid phosphor-derivedsample displayed the excitation-independent emission, implying its relatively simplechemical environment. All the three samples have good photostability and are stablein a solution at high ionic strength of5M. NaCl. In the HeLa cell survival test, all thecarbogenic nanoparticles exhibited low cytotoxicity. Especially in the highconcentration, the performance of all the samples were superior to that of thetraditional quantum dots, which render them better prospects for the biologicallabeling. In the following cell imaging to human embryonic kidney cells, all thesamples enter into cells without any further functionalization, and exhibit obviousphotoluminescence signal. In particular, the solid phosphor-derived sample penetratedinto the karyon without the modification with specific transferrable protein, and usingits fluorescence property, it is possible track the carbogenic nanoparticles. All thebiological results indicates that the three samples of carbogenic nanoparticles is ableto used as fluorescent probe molecules in cellular imaging and bio-detection.Moreover, there is no distinct difference in the photoluminescence property,cytotoxicity, and cell labeling results of these two kinds of defoliation-derivedcarbogenic nanoparticles, suggesting that the aqueous route we used for thepreparation of water soluble carbogenic nanoparticles is generally universal, and maybe extended to various defoliations.
In chapter four, the elemental zinc was introduced into the cages of microporousmagnesium-aluminophosphate and silicoaluminophosphate molecular sieve,respectively, using the designed vacuum chemical vapor reaction system. Elementalzinc reacted with the proton in the framework and the univalent zinc was generated.For the magnesium-aluminophosphate system, the formation of univalent zinc leadedthe dephosphorization on the framework. The removed phosphorus reacted withpartial univalent zinc, and generated zinc phosphide. We use the zincphosphide-loaded composite material as the evaporation source to synthesize a seriesof low-dimensional nanostructures of zinc phosphide on one substrate, includingnanoparticles, nanowires, and dense zinc phosphide films. The results show that thegrowth of zinc phosphide nanostructures follows the vapor-solid mechanism. On theother hand, for the silicoaluminophosphate system, ammonia molecules areintroduced into the univalent zinc-contained molecular sieve in sequence. At roomtemperature, the univalent zinc reacted with ammonia, resulting in zinc nitride in themicroporous, and the reaction is exothermic. The resulted zinc nitride-loadedmicroporous composite material displayed a certain room temperaturephotoluminescence. Since the high temperature or complicated equipment is alwaysneeded in its preparation, zinc nitride directly synthesized from ammonia at roomtemperature have not been achieved yet prior to our work.
引文
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