新型碳基有序介孔材料的合成、功能化及性质与应用

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作者：吴张雄 论文级别：博士 学科专业名称：无机化学 中文关键词：介孔碳材料 ; 模板合成 ; 石墨化 ; 表面功能化 ; 碳基复合材料 ; 氧化铝材料 ; 吸附与分离 英文关键词：mesoporous carbon materials ; templating synthesis ; graphitization ; surface functionalization ; carbon-based composites ; alumina ; adsorption and separation 学位年度：2011 导师：赵东元 学科代码：070301 学位授予单位：复旦大学 论文提交日期：2011-04-13

摘要

有序介孔材料具有尺寸均一且相互贯通的孔道体系,它们与原子、离子、分子乃至更大的客体之间的相互作用不仅仅局限于外表面,而更重要的是贯穿整个材料内部。这种性质使介孔材料成为当前化学与材料科学等的一大研究热点。纵观其近20年的发展历程,介孔材料的组成、结构、形貌以及孔性质等方面均方便可调。然而,目前为止,最有望实现规模化生产与实际工业应用的介孔材料是二氧化硅和碳。特别是,介孔碳材料具有巨大的比表面积、均一可调的介孔孔径以及良好的稳定性和导电性,在吸附与分离、催化、气体储存、电化学能量储存与转化、乃至生物医药等众多领域均具有广阔的应用前景。因此,本论文以碳基介孔材料作为研究对象。
     介孔碳材料的合成技术已经比较成熟,人们利用模板法合成了多种具有不同结构与形貌的介孔碳材料。然而,这类碳材料在以下几大方面还有待进一步研究：(1)大规模的合成技术；(2)介孔骨架的进一步晶化；(3)功能化表面或骨架的精细调控；(4)可商品化应用性质的开发。特别是对于通过软模板法合成的介孔碳材料,有关以上方面的研究正处于一个兴起阶段。本论文力求充分考虑当今介孔材料的研究前沿与发展趋势,根据实际应用需求,围绕介孔碳材料的合成、表面功能化、高分散与高活性纳米颗粒的嵌入、功能型纳米复合材料的构建以及以碳为模板合成其他介孔材料等方面展开了比较系统的研究工作；同时,论文针对性地研究了这些材料在水处理、气体储存以及电化学等方面的应用潜能。
     论文的第二章考虑纯碳材料的骨架性质。我们以二氧化硅为模板,甲烷为新型碳源,通过化学气相沉积,发展了一条简便省时的途径,可合成具有高石墨化程度的介孔碳材料。该合成过程不需任何载气,不需前驱体的填充；且甲烷热解的积碳速率快。因此合成快速,介孔碳的产量高。通过控制模板的类型、气相沉积的温度、时间等因素,碳材料的结构(p6m、Ⅰa3d等)、比表面积(200～1200 m2/g),孔体积(0.2-2.2 cm3/g)以及墙壁结晶程度等均简单可调。这类介孔碳材料具有较高的热稳定性,在900-1200℃进一步热处理可明显提高碳骨架的石墨结晶度,并维持良好的介观有序性和高孔隙率。这类材料由于其较高的比表面积、大的孔容以及高石墨结晶度,可作为锂离子电池电极材料,显示出良好的性能。
     论文的第三章考虑碳材料的表面性质。在不同的湿法氧化条件下,我们首次研究了介孔碳FDU-15孔性质的演化、结构稳定性以及表面含氧基团种类与含量的变化。该类介孔碳材料具有很高的抗氧化稳定性,远优于硬模板法合成的CMK-3。氧化后,碳材料孔道表面生成了大量的含氧基团(特别是羧基)；比表面积下降,主要归因于介孔墙壁中部分微孔被含氧基团堵塞；表面氧化后,材料在水溶液中的分散性具有较大的改善,在重金属离子的吸附与分离方面都显示出优良的性能。另外,利用三聚氰胺为氮源,我们发展了一条简单的热处理方法,可在FDU-15型介孔碳材料孔道或骨架中引入高浓度的含氮组分或基团。在较低的温度(～500℃)下处理,氮含量高达20.6 wt%。在700～900℃处理,氮含量也可达～4.5 wt%。含N物种或基团高度且均匀地分布在整个碳材料中,使该类材料在重金属离子以及CO2的吸附与分离应用中显示出较好的性能。
     论文的第四章考虑介孔碳材料的掺杂。我们以嵌段共聚物为模板,通过碳源、钙源与模板的一步共组装得到了负载CaO纳米颗粒的介孔碳材料。材料的孔隙率、CaO的含量及颗粒大小均简单可调。复合材料具有较高的比表面积(～1058 m2/g)和高含量(～20 wt%)、高分散且粒径小的CaO纳米颗粒,在CO2的吸附与分离方面显示出优异的性质。在低温范围(0～150℃),材料依靠比表面积高容量地吸附CO2(～7 mmol/g);在高温段(250～600℃),高分散的CaO纳米颗粒通过化学反应高容量且快速地捕捉CO2(～3.2 mmol/g,化学吸附在～3 min内完成)。此外,由于介孔的限域效应,CaO纳米颗粒的烧结受到较大的限制,复合材料对CO2化学吸附的循环稳定性得到了较大的改善。这类材料是首次报道的在大范围温度内均显示出良好CO2吸附性能的新型吸附剂。
     论文的第五章考虑碳基复合材料的合成。我们以二氧化硅为模板、CH4或CH4/H2为还原渗碳气氛、杂多酸为前驱体,首次在纳米尺度下协同地构建了一种新颖的具有类铂性质的介孔碳化钨/碳复合材料。由于前驱体转化到碳化钨的体积收缩很大,很难得到具有单一碳化钨骨架的介孔材料。我们巧妙地利用碳作为纳米连接,在还原渗碳反应的同时,将前驱体转化到碳化物产生的空隙原位积碳,从而很好地连接、稳定碳化钨纳米晶。复合材料具有很高的比表面积(～169 m2/g),高于文献报道的碳化钨纳米结构材料。我们系统地研究了模板的种类、孔径大小、前驱体用量以及渗碳反应的温度等对合成的影响,得到了一系列具有不同结构、碳含量以及孔性质的复合材料。
     在论文的第六章,通过精细调控,我们合成了一类结构新颖、性能优良的磁性氧化铁/碳复合材料。我们选用软模板法合成的具有双介孔(2.3,5.9 nm)分布的碳材料为模板,经适当氧化引入表面含氧基团后,通过一步填充便可在碳材料孔道中引入高含量的超顺磁性氧化铁纳米粒子(～40 wt%),纳米颗粒高度且均匀地分散在整个介孔中。复合材料仍保持高比表面积(～1000 m2/g)；同时,由于纳米颗粒主要负载在碳材料的主介孔孔道中,其墙壁上的小介孔使整个孔道体系保持开放,有利于客体分子的快速传输。以上性质使复合材料对砷具有优异的吸附与分离性能。其吸附容量非常高(达～30 mg/g)；吸附速度快非常快,属于准二级动力学吸附过程。此外,温度、pH、氧化铁含量等对吸附的影响得到了较为详细的研究,最佳的吸附温度和pH值分别为35℃和7。此外,该合成方法具有普适性,可合成一系列负载高分散纳米颗粒的碳基复合材料。
     在论文的第七章,我们进一步利用碳材料表面含氧基团功能化带来的优势,开创性地以软模板法合成的介孔碳材料为模板,合成了一系列孔道构造、孔径与孔隙率均可调的有序介孔氧化铝材料。我们选取具有双介孔(2.3,5.9 nm)分布的碳材料为模板,经适当氧化引入表面含氧基团后,通过调节硝酸铝的填充量,可方便地控制氧化铝在碳模板中的装载量从零开始到只填入碳模板的小介孔,再到小介孔填满而主介孔达到不同程度的填充度。由此,可在较大的范围内控制最终氧化铝材料的孔径(3.6-10 nm)、比表面积(158～450 m2/g)和孔体积(0.17～1.2 cm3/g).该方法首次报道以单一介孔碳材料为模板同时合成了具有正相和反相两种孔道构造的有序介孔材料。此外,该方法可以扩展到其他金属氧化物(如氧化镁)介孔材料的合成。
Ordered mesoporous materials (OMMs) possess regular, uniform and interpenetrating mesopores. Compared with their bulk counterparts, they can interact with atoms, ions, molecules or even larger guest spices not only at the external surface, but also through the whole internal pore system, which makes them one of the research hot spots in chemistry and material science. After a two-decade development, mesoporous materials with tunable framework compositions, mesostructures, morphologies and porosities can be easily obtained. Presently, OMMs that tend to be most possible for large-scale production and practical application are silica and carbon materials. Among them, mesoporous carbon materials hold several fascinating properties including high specific surface areas, uniform and tunable mesopores, good chemical and thermal stability and electric conductivity, showing promising potential for adsorption and separation, catalysis, gas storage, energy storage and conversion as well as delivery of biomolecules. As such this thesis mainly focuses on the synthesis and application of mesoporous carbon and carbon-based materials.
     A larger number of ordered mesoporous carbon materials (OMCs) with different mesostructures, morphologies and porosities can be obtained through either hard or soft-templating methods, which have been fairly developed since 1999. However, there are still several challenging issues that need further investigation, including, (1) synthetic methods for large-scale production, (2) further graphitization of carbon framework, (3) fine control of either surface or framework functionality and (4) exploration of practical application. Research activities regarding the above issues are still limited especially for the OMCs fabricated through soft-templating. Through rational consideration of the research frontiers and possible requirements in practical applications of OMCs, this thesis presents a systematic study regarding the following well-connected aspects of OMCs, including graphitization, surface functionalization, framework modification, novel composites construction, synthesis of metal oxides with OMCs as hard templates, and their applications in water treatment, gas storage, etc.
     In Chapter 2, a new route has been developed to fabricate a series of OMCs with highly graphitized mesopore walls by using mesoporous silica materials as hard templates, methane as a new carbon precursor and chemical vapour deposition at 700～1000℃for carbon loading. The synthesis procedure is quite simple and time-saving without any carrying gas or impregnation step. Meanwhile, the rate of carbon deposition through thermal decomposition of methane is fast so that large quantities of OMCs can be obtained within a short time. Through adjusting several factors including different silica templates, various deposition temperatures and durations, the mesostructure (p6m, laid etc.), surface area (200～1200 m2/g), pore volume (0.2～2.2 cm3/g) and graphitization degree of the final OMCs can be easily manipulated. The prepared OMCs show good thermal stability, with a further improved graphitization degree upon a thermal treatment at 900～1200℃under vacuum condition. Due to their high surface area, large pore volume and graphitic nature, these OMCs can be adopted as electrodes in lithium ion batteries, showing good performance with high reversible capacity and good cyclic stability.
     In Chapter 3, the pore evolution, mesostructure stability and simultaneous surface functionalization with oxygen-containing groups of FDU-15 under different wet oxidation conditions (different oxidants, various temperature and periods) are systematically investigated for the first time. The OMC FDU-15 shows overwhelmingly better stability than the mesostructural analogue CMK-3. Upon oxidation, high concentration of surface oxygen-containing groups, especially carboxylic groups, can be readily generated, which make the carbon materials hydrophilic and dispersible in aqueous environment. After oxidation, the surface area and pore volume of the carbon material both decrease to a large extent, which are mainly due to the reduction of microporosity because a large proportion of micropores are blocked by the surface oxides. The surface functionalized carbon material shows highly promising performance for immobilization of heavy metal ions, basic dyes and biomolecules. On the other hand, a new and simple pathway has been explored to introduce nitrogen-containing functionalities onto the surface of soft templated OMCs with melamine as a precursor. The final content of nitrogen can be easily controlled by simply impregnating OMCs with melamine and heating the composites at different temperature (500～900℃). Under a low temperature (～500℃), the nitrogen content can be achieved to～20.6 wt%, with carbon nitride as a major contribution, while the nitrogen content significantly drops down to～2.0 wt% with the increase of temperature to 700～900℃. The nitrogen-containing functionalities are highly and uniformly dispersed in the whole carbon frameworks, rendering the carbon materials very attracting adsorbents for heavy metal ion removal and CO2 capture.
     In Chapter 4, novel ordered mesoporous calcium oxide/carbon (CaO/C) composite materials are obtaied through one-pot co-assenbly of resol, calcium nitrate and surfactant. The porosity, CaO content as well as the particle size can be easily tuned by varying the molar ratio between the carbon and calcium precursors and the carbonization temperature. With high specific surface areas (up to～1058 m2/g), high contents of CaO (up to～20 wt%) of uniform dispersion and small particle size, the composite materials delivery highly attracting properties for CO2 adsorption and separaton over a wide range of temperatures (0～600℃). At a low temperature range (0～150℃), the composite materials can uptake CO2 with high capacities (up to～7 mmol/g) though physisorption. At a high temperature range (250～600℃癈), high CO2 uptake capacities (up to 3.2 mmol/g) can be still achieved through chemisorption based on the rection between CaO nanoparticels and CO2. The CaO nanoparticle are fully available and can be completely converted to carbonate within 3 mins at～450℃due to the high activity of the small CaO nanopartices. Besides, due to the confiment effect in the nanopore space, the sintering of CaO nanopartices during CO2 chemisorption is significantly restricted, leading to a much improved cyclic stability during CO2 chemisorptipon and sorbent regeneration.
     In Chapter 5, for the first time, a novel ordered mesoporous tungsten carbide/carbon (WC/C) composite with platinum-like behavior is cooperatively constructed at a nano-scale by hard-templating method with silica as the template, tungsten heteropolyacid as the precursor, and methane or methane/hydrogen mixtrue as a reduction and carburization agent. Tungsten heteropolyacid is first loaded into the mesopores of silica template, followed by thermal decompostion, reduction and carburization, which convert the precursor into WC. The large pore volume released during the conversion is simultaneously occupied by deposited carbon which can stabilize and connect the WC nanocrystals to form continuous nanowires and support the ordered mesostructure. The WC/C composites hold high specific surface (up to 169 m2/g), much larger than any other reported WC nanostructured materials. The influcing factors including different silica template, pore size of the template, precursor loading level and carburization temperature are systematically studied, allowing the successful synthesis of a series of WC/C composites with different mesostructures (p6m,Ⅰa3d, etc.), surface areas (80～170 m2/g) and free carbon amounts (15～50 wt%).
     In Chapter 6, ordered mesoporous magnetic iron oxide/carbon (Fe2O3/C) composites with novel nanostructures and excellent performance for arsenic removal have been rationally designed and fabricated. A surface functionalized mesoporous carbon with bimodel mesopores (2.3 and 5.9 nm) obtained from soft-templating is adopted as a template and iron nitrate as the precursor. With a simple impregnation step followed by calcination, very high contents (up to 40 wt%) of y-Fe2O3 nanoparticles can be loaded into the main mesopores (5.9 nm), with the nanoparticles highly and uniformly dispersed in the whole carbon matrix. On the other hand, the empty small mesopores (2.3 nm) maintain a high surface area (up to～1000 m2/g) and keep the whole pore system quite open, which can facilitate the diffusion and transportation of guest molecules. As a result, these composite materials show excellent performance for arsenic removal, with very high adsorption capacities (up to 30 mg/g), fast adsorption rate (peseudo-second order kinetics), ready magnetic separation and good cyclic stability. Besides, several influencing factors on arsenic removal including temperature, pH value and content of iron oxide are studied in detail, with a best adsorption temperature and pH value of about 35℃and 7, respectively. Finally, the synthesis method is versatile for loading a series of other nanoparticulate metal oxide into the pore system of the carbon matrix.
     In Chapter 7, an efficient route is developed for controllable synthesis of ordered mesoporous alumina (OMA) materials with variable pore architectures and high mesoporosity, as well as crystalline framework. The route is based on the nanocasting pathway with a bimodal mesoporous (2.3,5.9 nm) carbon as the hard template. The method here first realizes the possibility of creating two ordered mesopore architectures by using a single carbon hard template obtained from organic-organic self-assembly, which is also the first time that such carbon materials are adopted to replicate ordered mesoporous materials. The bimodal mesopores and the surface oxygen-containing functionalities make it possible to selectively load alumina into the small mesopores dominantly and/or with a layer of alumina coated on the inner surface of the large mesopores with different thicknesses until a full loading achieved. Thus, OMA materials with variable pore architectures (similar and reverse mesostructures relative to the carbon template) and controllable surface areas (158～450 m2/g), pore volumes (0.17～1.2 cm3/g) and pore sizes (3.6～10 nm) are achieved. Furthermore, our method is versatile enough to be used for general synthesis of other important but difficult-to-synthesize mesoporous metal oxides, such as magnesium oxide.

引文

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