介孔纳米晶体金属氧化物材料的制备、表征及性能研究
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摘要
本文以室温长链咪唑溴离子液体(Cnmim+Br-,n=8,12,14,16)为模板剂,通过软模板法合成了具有高热稳定性的介孔纳米晶体氧化锡材料,并在此基础上通过软模板法和固液技术相结合,合成了具有高比表面、高热稳定性及高结晶性的介孔氧化锆和氧化钛材料。利用X射线粉末衍射(XRD)、高分辨透射电镜(HRTEM)、氮气吸附-脱附、红外傅立叶变换(IR-FT)、热重-差热分析(TG-DTA)和热重-差示扫描量热分析(TG-DSC)等技术,研究了以下内容：
以长链咪唑溴为模板剂,锡酸钠为无机前驱体通过软模板法合成了具有高热稳定性(焙烧温度达700℃)的介孔纳米晶体氧化锡材料。高分辨电镜和氮气吸附脱附分析结果表明该材料具有短程有序的介孔结构,比表面和孔径分别为350m2／g和2.2 nm,孔壁氧化锡纳米晶粒尺寸为2.5 nm。红外分析结果表明,模板剂离子液体与传统的阳离子表面活性剂如十六烷基三甲基溴化铵(CTAB)相比,在与无机前驱体组装过程中其荷正电的咪唑头基与荷负电的氧化锡前驱体之间的相互作用力除了传统的静电作用外,还具有氢键作用,同时,咪唑环之间存在π-π堆积作用,正是基于这些独特的相互作用提高了介孔氧化锡材料的热稳定性。另外,氧化锡材料介孔结构的有序性主要受模板剂的链长、模板剂与氧化锡前驱物的摩尔比例、反应过程的pH值及焙烧温度等因素的影响。
以长链咪唑溴(C16mim+Br-)为模板剂,硫酸锆为无机前驱体,通过软模板法和固液技术相结合(软模板-固液技术)的新策略合成了具有高比表面的介孔纳米晶体氧化锆材料。该策略是利用固液技术将具有低熔点的金属硝酸盐客体填充到软模板法合成的有序介观相氧化锆杂化物主体中,高温焙烧后通过刻蚀孔道内的金属氧化物,最终得到了介孔纳米晶体氧化锆材料。广角XRD分析结果表明客体硝酸镁盐与主体氧化锆杂化材料研磨混合后,在高于熔点(>95℃)时其熔液通过毛细作用能够渗入到作为主体的氧化锆杂化材料的介孔孔道中(其最大渗入量达到约50%(w／w))。TG-DTA分析结果表明随焙烧温度的升高,硝酸镁盐的热分解在孔道内提供了氧化气氛(O2)和硬支撑(MgO),促使模板剂在较低的温度下分解完全,抑制了孔壁氧化锆纳米晶粒的过快生长,避免孔道坍塌。X射线能谱(EDX)分析结果表明在盐酸溶液刻蚀后,镁元素没有掺入到氧化锆骨架中,避免硬模板法在氧化锆骨架中掺入了较多的硅元素。高分辨电镜和氮气吸附脱附分析结果表明在600℃焙烧后氧化锆材料具有蠕虫状介孔结构,孔壁由尺寸约为2.3nm的四方相氧化锆纳米晶粒组成,比表面为255m2／g,孔径为4.3nm。相反,通过单一软模板法直接焙烧后合成的氧化锆材料在相同的焙烧温度,比表面仅为9.5 m2／g。最后,所合成的介孔氧化锆材料展示了紫外荧光特性。
以长链咪唑溴(C16mim+Br-)为模板剂,硫酸钛为无机前驱体,通过软模板-固液技术策略合成了孔壁具有混合晶相的介孔纳米晶体氧化钛材料。广角XRD分析结果表明作为客体的硝酸镁盐通过固液技术渗入到作为主体被模板剂占据的介孔孔道中；TG-DTA分析结果表明在焙烧过程中,在孔道内客体硝酸镁盐的热分解既能促使模板剂在更低的温度分解完全又提供了必要的硬支撑(MgO),抑制了氧化钛纳米晶粒的快速生长,避免孔道坍塌。广角XRD和拉曼分析结果表明孔道中MgO的存在促使孔壁氧化钛晶相由锐钛相向板钛相和金红石相转变,并且随焙烧温度的提高板钛相含量逐渐增加。高分辨电镜和氮气吸附脱附分析结果表明在600℃焙烧后氧化钛材料具有蠕虫状介孔结构,比表面为255m2／g,孔径为4.1nm。相反,通过单一软模板法直接焙烧后合成的氧化钛材料在相同的焙烧温度,比表面仅为64m2／g。光催化甲基橙结果表明,所合成的介孔氧化钛材料的光催化能力由比表面和晶相组成决定。
In this thesis, mesoporous nanocrystalline tin oxide materials with high thermal stability were synthesized via the soft-templating method, using long-chain ionic liquids 1-alkyl-3-methylimidazolium bromide (Cnmim+Br-,n= 8,12,14,16) as templates. And also, mesoporous zirconia and titania materials with high BET specific surface area, high thermal stability and high crystallinity were also fabricated via combining the soft-templating with solid-liquid method (CSSL). The resulting samples were mainly characterized by X-ray powder diffraction (XRD), High resolution transmission electron microscopy (HRTEM), Nitrogen adsorption-desorption, Fourier transform infrared spectrometer (FT-IR) and Thermal analyses.
Using 1-alkyl-3-methylimidazolium bromide (Cnmim+Br-, n= 8,12,14,16) as templates and sodium stannate as precursors, mesoporous nanocrystalline tin oxide materials with high thermal stability (up to 700℃) were synthesized via the soft-templating method. The HRTEM and Nitrogen adsorption-desorption results indicated that the obtained mesoporous tin oxide with ordered mesoporous structure in short range possessed high specific surface area (ca.350 m2/g). The pore walls were composed of tin oxide nanocrystallites with size of ca.2.5 nm. The FT-IR analysis showed that the high thermal stability for the obtained mesoporous tin oxide was attributed to the wide interaction between the templating agent C16mim+Br-molecules and tin oxide. It involved the electrostatic interaction and H-bonding between C16mim+Br- molecules and tin oxide, as well asπ-πstacking between the imidazolium rings. In addition, the ordered mesostructures were influenced by the reaction conditions, such as pH values of the hydrolysis of tin salt, the different chain lengths of RTILs and different calcination temperatures.
A novel strategy involving the combination of soft-templating and solid-liquid method (CSSL) was designed to synthesize mesoporous nanocrystalline zirconia with high specific surface area. The mesostructured zirconia hybrid was firstly synthesized via cooperative assembly between zirconium sulphate as inorganic precursor and 1-hexadecyl-3-methylimidazolium bromide (C16mim+Br-) as the structure-directing agent, and subsequently ground with solid magnesium nitrate salt followed by heat-treatment in air. Finally, after high-temperature calcination, the mesoporous nanocrystalline zirconia materials were obtained after etching the metal oxide inside the porous channels. The wide-angle XRD results indicated that Mg (NO3)2·6H2O salt transforming into liquid state could infiltrate into the pore channels occupied by templates and be well dispersed in the mesostructured zirconia hybrid when it was heated above its melting point (95℃). The maximum amount of the guest inside the host was 50%(w/w). The TG-DTA analysis suggested that the thermal decomposition of Mg(NO3)2-6H2O salt provided the oxidative atmosphere (O2) and hard pillaring-agent (MgO) inside the pore channels, which contributed to the full decomposition of the templates at low temperature, and the restriction of the quick growth of ZrO2 nanocrystallites in the pore walls, avoiding the collapse of the mesopores. The EDX results showed that the magnesium could not penetrate into the zirconia framework after the impregnation with 10 wt% HCl. On the contrary, more silicon elements could penetrate into the zirconia framework if the hard-templating method was used. The HRTEM and Nitrogen adsorption-desorption results indicated that the zirconia material after calcination at 600 C possessed a wormlike arrangement of mesopores surrounded by tetragonal ZrO2 nanocrystallites of ca.2.3 nm. The BET surface area was 255 m2/g and the pore size was ca.4.3 nm. Contrastingly, as for the sample synthesized via the single soft-templating method, the BET surface area was only 9.5 m2/g. Moreover, the obtained mesoporous zirconia materials exhibited excellent fluorescence features.
Mesoporous anatase-brookite nanocrystalline titania was synthesized via the strategy relying on the combination of soft-templating and solid-liquid method (CSSL), using titanium sulphate as precursor and 1-hexadecyl-3-methylimidazolium bromide (C16mim+Br-) as structure-directing agent. The wide-angle XRD results indicated that relying on the solid-liquid method, the magnesium nitrate salt as guest could infiltrate into the pore channels occupied by the templates inside the mesostructured titania hybrid as host. The TG-DTA analysis suggested that the thermolysis of Mg(NO3)2·6H2O salt inside pore channels as guest could not only induce the complete decomposition of the templates at low temperature, but also provide the essential hard-pillaring agent (MgO), resulting in the restriction of the quick growth of the nanocrystalline titania in the pore walls and avoiding the collapse of the mesopores. The XRD and Raman results showed that MgO retaining on the surface of the titania framework induced the phase transformation from anatase phase to brookite and rutile phases, and the amount of the brookite phase increased as the temperature rose. The HRTEM and Nitrogen adsorption-desorption results indicated that the titania material after calcination at 600℃possessed a wormlike arrangement of mesopores. The BET surface area was 255 m2/g, and the pore size was ca.4.1 nm. Contrastingly, as for the sample synthesized via the single soft-templating method, the BET surface area was only 64 m2/g. Moreover, the photocatalytic activities of the resulting titania materials in the degradation of methylene orange under UV irradiation were found to be determined by their surface areas and crystal phase contents.
以长链咪唑溴为模板剂,锡酸钠为无机前驱体通过软模板法合成了具有高热稳定性(焙烧温度达700℃)的介孔纳米晶体氧化锡材料。高分辨电镜和氮气吸附脱附分析结果表明该材料具有短程有序的介孔结构,比表面和孔径分别为350m2／g和2.2 nm,孔壁氧化锡纳米晶粒尺寸为2.5 nm。红外分析结果表明,模板剂离子液体与传统的阳离子表面活性剂如十六烷基三甲基溴化铵(CTAB)相比,在与无机前驱体组装过程中其荷正电的咪唑头基与荷负电的氧化锡前驱体之间的相互作用力除了传统的静电作用外,还具有氢键作用,同时,咪唑环之间存在π-π堆积作用,正是基于这些独特的相互作用提高了介孔氧化锡材料的热稳定性。另外,氧化锡材料介孔结构的有序性主要受模板剂的链长、模板剂与氧化锡前驱物的摩尔比例、反应过程的pH值及焙烧温度等因素的影响。
以长链咪唑溴(C16mim+Br-)为模板剂,硫酸锆为无机前驱体,通过软模板法和固液技术相结合(软模板-固液技术)的新策略合成了具有高比表面的介孔纳米晶体氧化锆材料。该策略是利用固液技术将具有低熔点的金属硝酸盐客体填充到软模板法合成的有序介观相氧化锆杂化物主体中,高温焙烧后通过刻蚀孔道内的金属氧化物,最终得到了介孔纳米晶体氧化锆材料。广角XRD分析结果表明客体硝酸镁盐与主体氧化锆杂化材料研磨混合后,在高于熔点(>95℃)时其熔液通过毛细作用能够渗入到作为主体的氧化锆杂化材料的介孔孔道中(其最大渗入量达到约50%(w／w))。TG-DTA分析结果表明随焙烧温度的升高,硝酸镁盐的热分解在孔道内提供了氧化气氛(O2)和硬支撑(MgO),促使模板剂在较低的温度下分解完全,抑制了孔壁氧化锆纳米晶粒的过快生长,避免孔道坍塌。X射线能谱(EDX)分析结果表明在盐酸溶液刻蚀后,镁元素没有掺入到氧化锆骨架中,避免硬模板法在氧化锆骨架中掺入了较多的硅元素。高分辨电镜和氮气吸附脱附分析结果表明在600℃焙烧后氧化锆材料具有蠕虫状介孔结构,孔壁由尺寸约为2.3nm的四方相氧化锆纳米晶粒组成,比表面为255m2／g,孔径为4.3nm。相反,通过单一软模板法直接焙烧后合成的氧化锆材料在相同的焙烧温度,比表面仅为9.5 m2／g。最后,所合成的介孔氧化锆材料展示了紫外荧光特性。
以长链咪唑溴(C16mim+Br-)为模板剂,硫酸钛为无机前驱体,通过软模板-固液技术策略合成了孔壁具有混合晶相的介孔纳米晶体氧化钛材料。广角XRD分析结果表明作为客体的硝酸镁盐通过固液技术渗入到作为主体被模板剂占据的介孔孔道中；TG-DTA分析结果表明在焙烧过程中,在孔道内客体硝酸镁盐的热分解既能促使模板剂在更低的温度分解完全又提供了必要的硬支撑(MgO),抑制了氧化钛纳米晶粒的快速生长,避免孔道坍塌。广角XRD和拉曼分析结果表明孔道中MgO的存在促使孔壁氧化钛晶相由锐钛相向板钛相和金红石相转变,并且随焙烧温度的提高板钛相含量逐渐增加。高分辨电镜和氮气吸附脱附分析结果表明在600℃焙烧后氧化钛材料具有蠕虫状介孔结构,比表面为255m2／g,孔径为4.1nm。相反,通过单一软模板法直接焙烧后合成的氧化钛材料在相同的焙烧温度,比表面仅为64m2／g。光催化甲基橙结果表明,所合成的介孔氧化钛材料的光催化能力由比表面和晶相组成决定。
In this thesis, mesoporous nanocrystalline tin oxide materials with high thermal stability were synthesized via the soft-templating method, using long-chain ionic liquids 1-alkyl-3-methylimidazolium bromide (Cnmim+Br-,n= 8,12,14,16) as templates. And also, mesoporous zirconia and titania materials with high BET specific surface area, high thermal stability and high crystallinity were also fabricated via combining the soft-templating with solid-liquid method (CSSL). The resulting samples were mainly characterized by X-ray powder diffraction (XRD), High resolution transmission electron microscopy (HRTEM), Nitrogen adsorption-desorption, Fourier transform infrared spectrometer (FT-IR) and Thermal analyses.
Using 1-alkyl-3-methylimidazolium bromide (Cnmim+Br-, n= 8,12,14,16) as templates and sodium stannate as precursors, mesoporous nanocrystalline tin oxide materials with high thermal stability (up to 700℃) were synthesized via the soft-templating method. The HRTEM and Nitrogen adsorption-desorption results indicated that the obtained mesoporous tin oxide with ordered mesoporous structure in short range possessed high specific surface area (ca.350 m2/g). The pore walls were composed of tin oxide nanocrystallites with size of ca.2.5 nm. The FT-IR analysis showed that the high thermal stability for the obtained mesoporous tin oxide was attributed to the wide interaction between the templating agent C16mim+Br-molecules and tin oxide. It involved the electrostatic interaction and H-bonding between C16mim+Br- molecules and tin oxide, as well asπ-πstacking between the imidazolium rings. In addition, the ordered mesostructures were influenced by the reaction conditions, such as pH values of the hydrolysis of tin salt, the different chain lengths of RTILs and different calcination temperatures.
A novel strategy involving the combination of soft-templating and solid-liquid method (CSSL) was designed to synthesize mesoporous nanocrystalline zirconia with high specific surface area. The mesostructured zirconia hybrid was firstly synthesized via cooperative assembly between zirconium sulphate as inorganic precursor and 1-hexadecyl-3-methylimidazolium bromide (C16mim+Br-) as the structure-directing agent, and subsequently ground with solid magnesium nitrate salt followed by heat-treatment in air. Finally, after high-temperature calcination, the mesoporous nanocrystalline zirconia materials were obtained after etching the metal oxide inside the porous channels. The wide-angle XRD results indicated that Mg (NO3)2·6H2O salt transforming into liquid state could infiltrate into the pore channels occupied by templates and be well dispersed in the mesostructured zirconia hybrid when it was heated above its melting point (95℃). The maximum amount of the guest inside the host was 50%(w/w). The TG-DTA analysis suggested that the thermal decomposition of Mg(NO3)2-6H2O salt provided the oxidative atmosphere (O2) and hard pillaring-agent (MgO) inside the pore channels, which contributed to the full decomposition of the templates at low temperature, and the restriction of the quick growth of ZrO2 nanocrystallites in the pore walls, avoiding the collapse of the mesopores. The EDX results showed that the magnesium could not penetrate into the zirconia framework after the impregnation with 10 wt% HCl. On the contrary, more silicon elements could penetrate into the zirconia framework if the hard-templating method was used. The HRTEM and Nitrogen adsorption-desorption results indicated that the zirconia material after calcination at 600 C possessed a wormlike arrangement of mesopores surrounded by tetragonal ZrO2 nanocrystallites of ca.2.3 nm. The BET surface area was 255 m2/g and the pore size was ca.4.3 nm. Contrastingly, as for the sample synthesized via the single soft-templating method, the BET surface area was only 9.5 m2/g. Moreover, the obtained mesoporous zirconia materials exhibited excellent fluorescence features.
Mesoporous anatase-brookite nanocrystalline titania was synthesized via the strategy relying on the combination of soft-templating and solid-liquid method (CSSL), using titanium sulphate as precursor and 1-hexadecyl-3-methylimidazolium bromide (C16mim+Br-) as structure-directing agent. The wide-angle XRD results indicated that relying on the solid-liquid method, the magnesium nitrate salt as guest could infiltrate into the pore channels occupied by the templates inside the mesostructured titania hybrid as host. The TG-DTA analysis suggested that the thermolysis of Mg(NO3)2·6H2O salt inside pore channels as guest could not only induce the complete decomposition of the templates at low temperature, but also provide the essential hard-pillaring agent (MgO), resulting in the restriction of the quick growth of the nanocrystalline titania in the pore walls and avoiding the collapse of the mesopores. The XRD and Raman results showed that MgO retaining on the surface of the titania framework induced the phase transformation from anatase phase to brookite and rutile phases, and the amount of the brookite phase increased as the temperature rose. The HRTEM and Nitrogen adsorption-desorption results indicated that the titania material after calcination at 600℃possessed a wormlike arrangement of mesopores. The BET surface area was 255 m2/g, and the pore size was ca.4.1 nm. Contrastingly, as for the sample synthesized via the single soft-templating method, the BET surface area was only 64 m2/g. Moreover, the photocatalytic activities of the resulting titania materials in the degradation of methylene orange under UV irradiation were found to be determined by their surface areas and crystal phase contents.
引文
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