钴基核壳纳米结构材料及空心纳米结构的制备与性能研究
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摘要
在本论文中，采用液相化学方法(溶胶-凝胶法、均匀沉淀法、水热法)制备了核壳结构复合物。在制备核壳结构复合物的基础上，通过化学刻蚀的方法，除去内核模板，得到空心球，并且通过改变前驱体的浓度或反应时间，实现了对壳层厚度的控制。在合成的基础上进一步研究了核壳结构复合物的形成机理，以及介孔的形成机理，并讨论了它们的结构对其电化学性质、磁性质的影响。
1．介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物的合成与表征
利用文献报道的方法，首先制备了四氧化三钴纳米颗粒。然后，将四氧化三钴纳米颗粒分散在一定比例的乙醇-水-氨水-CTAB混合溶液中，加入前驱体TEOS，二氧化硅沉积在四氧化三钴超晶格颗粒的表面，形成介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物。根据广角XRD表征结果，在形成核壳结构复合物的过程中，四氧化三钴物的相未发生变化，表明四氧化三钴具有良好的化学稳定性和水热稳定性。低角度XRD表征结果表明，四氧化三钴和二氧化硅具有介观结构。通过改变前驱体TEOS的浓度，可以调节二氧化硅壳层的厚度(10-35nm)。电镜观察表明二氧化硅壳层的存在有效地抑制了高温下Co_3O_4纳米晶的生长。氮气吸附脱附测试结果表明介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物(壳层厚度：20nm)的比表面积为238.6m~2／g，其孔径呈现双模式介孔分布，最可几孔径尺寸分别为2.0nm和8.8nm。随着壳层厚度的增加，核壳纳米结构复合物的比表面积变大。用氢氟酸刻蚀介孔Co_3O_4／介孔SiO_2核壳结构纳米复合物，可以除去二氧化硅壳层，得到介孔四氧化三钴纳米颗粒。氮气吸附测试结果显示介孔四氧化钴的比表面积为86.4m~2／g，最可几孔径尺寸是8.7nm。实验结果证明核壳结构复合物的形成是源于荷负电的Co_3O_4纳米颗粒、荷正电的CTAB胶束、荷负电的水解聚硅酸根之间的静电引力。这为核壳结构复合物的合成及由纳米晶聚集形成的介孔材料的合成提供了一条新的路线。电化学测试结果表明，与未包覆的四氧化钴纳米颗粒相比，介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物显示出更高的放电容量，这是由于二氧化硅壳层抑制Co_3O_4纳米晶生长，导致复合物具有尺寸更小的Co_3O_4纳米晶的缘故。
2．介孔氢氧化亚钴纳米空心球的合成与表征
首先，采用文献报道的方法合成出二氧化硅纳米颗粒，颗粒尺寸约为75nm。然后，将一定量的二氧化硅纳米颗粒分散于去离子水中，分别加入一定比例的尿素、硝酸钴，在80℃进行回流，氢氧化亚钴沉积在二氧化硅纳米颗粒的表面，得到二氧化硅／介孔氢氧化亚钴核壳结构纳米复合物。用氢氧化钠溶液刻蚀二氧化硅／介孔氢氧化亚钴核壳纳米结构复合物，除去二氧化硅模板，得到介孔氢氧化亚钴空心球。通过改变反应时间，可以实现对介孔氢氧化亚钴纳米空心球壁层厚度的控制(10-25nm)。XRD表征表明氢氧化亚钴为无定形态。用0.5M的氢氧化钠溶解复合物中的二氧化硅，得到氢氧化亚钴纳米空心球。相应的低角度XRD谱图在2θ≈1.5°出现一宽的衍射峰，表明氢氧化亚钴空心球具有无序介孔结构，电镜观察表明介孔是由氢氧化亚钴纳米管而导致，这是首次利用液相技术制备具有均匀内直径的氢氧化亚钴纳米管。根据XPS表征结果，在复合物中，Co 2p的特征峰位于798.37eV和782.47eV，Co 2p_(1／2)和Co 2p_(3／2)的电子结合能间隔为15.9eV，证明复合物中钴是以氢氧化亚钴形式存在。根据氮气吸附测试的结果，氢氧化亚钴空心球(壁层厚度：10nm)的比表面积为418m~2／g，其最可几孔径尺寸为3.9nm，孔径尺寸的分布范围相对较窄。随着壁层厚度的增加，氢氧化亚钴空心球的比表面积减小。实验结果证明核壳结构复合物的形成是源于荷负电的二氧化硅纳米颗粒、荷正电的水合钴离子之间的静电引力，而氢氧化亚钴纳米管的形成则经历了氢氧化亚钴纳米颗粒——氢氧化亚钴纳米片层——氢氧化亚钴纳米管的变化过程。电化学测试结果表明，与块体氢氧化亚钴相比，该氢氧化亚钴纳米空心球电极材料显示出更高的比电容和循环稳定性，这是由于氢氧化亚钴纳米空心球具有更大的比表面积和较短的离子传输距离的缘故。
3．铁酸钴空心球的合成与表征
将葡萄糖-硫酸钴-硫酸亚铁铵的混合溶液进行水热处理，葡萄糖首先通过水热反应，形成微米级碳球。碳球的表面具有许多羟基，混合溶液中的Fe~(2+)、Co~(2+)能够直接吸附在碳球的表面，形成碳球／金属盐核壳结构复合物。通过焙烧处理除去碳球，得到铁酸钴空心球。XRD和EDS表征结果证实产物是铁酸钴。TEM和HRTEM观测的结果表明铁酸钴空心球的尺寸介于600nm-900nm之间，壁层厚度约为150nm。铁酸钴空心球由纳米晶聚集而成，纳米晶的尺寸约为28nm。磁性质测试结果表明，铁酸钴空心球具有铁磁性。其饱和磁化强度为54emu／g，小于块体铁酸钴的饱和磁化强度(72emu／g)。这是由于铁酸钴空心球为纳米晶聚集体，具有表面效应和小颗粒尺寸效应的缘故。铁酸钴空心球的矫顽力为860Oe，剩余磁化强度是18emu／g。该材料具有较高的磁饱和强度和矫顽力。这种表面亲水的材料具有生物相容性，在药物传输方面具有潜在的应用价值。
In this paper, the core-shell nanostructures were prepared using simple liquid chemical methods (sol-gel method; homogeneous precipitation method; hydrothermal method). On the basis of this composite, the hollow sphere was obtained after the core template was removed by chemical etching or calcination. The shell thickness could be controlled by changing the concentration of precursor or reaction time. Based on the experiment, the formation mechanisms of core-shell structure and the mesopores were studied. It was discussed how the structure has effect on its electrochemical properties or magnetic properties.
1. Fabrication and Characterization of Mesoporous Co_3O_4 Core/MesoporousSilica Shell Nanocomposites
The parent Co_3O_4 particles comprised of oriented-aggregated nanocrystals was firstly prepared followed our previous report. Then, the Co_3O_4 nanoparticles were dispersed in a certain proportion of ethanol-water-ammonia-CTAB mixture. After the addition of the precursor TEOS, the silica directly deposited on the surface of Co_3O_4 nanoparticles, and the mesoporous Co_3O_4/mesoporous silica core/shell nanocomposite was formed. Based on the wide-angle X-ray diffraction results, both of the bare Co_3O_4 nanoparticles and the coated Co_3O_4 nanoparticles exhibit the same spinel structure. So it is concluded that Co_3O_4 nanoparticles has good chemical stability and thermal stability. Based on the low-angle X-ray diffraction results, it is confirmed that the Co_3O_4 core and the silica shell have mesostructures. TEM observation indicates that the presence of the silica shell effectively prevents the Co_3O_4 nanocrystals from growing. The thickness of silica shell could be controlled by changing the concentration of precursor TEOS. Based on the experiments, the formation mechanism of the nanocomposite with a mesoporous silica shell and a mesoporous Co_3O_4 core was proposed, which is based on the electrostatic attraction between negatively charged parent Co_3O_4 particles, the positively charged CTAB micelles and the negatively charged silicate species. The mesoporous structure of the Co_3O_4 core and the silica shell has been further confirmed by the N_2 adsorption-desorption isotherm. This work might provide a novel route to core/shell nanostructures and the mesoporous materials from the aggregating of the nanocrystals. Electrochemical analysis reveals that the composite shows a relatively higher discharge capacity comparing to its corresponding bare Co_3O_4 nanoparticles.
2. Synthesis and Characterization of Mesoporous cobalt hydroxide nano-hollow sphere
Firstly, the silica nanoparticles were synthesized according to previous report. The average size of silica particles is about 75 nm. Then, a certain amount of silica nanoparticles were dispersed in deionized water. After the addition of the urea and cobalt nitrate, the solution was heated to 80℃, and refluxed at that temperature for 2 hours. As a result, the cobalt (II) hydroxide was deposited on the surface of silica, and the silica core/mesoporous cobalt (II) hydroxide shell nanocomposite was formed. On the basis of the nanocomposite, the mesoporous cobalt (II) hydroxide hollow sphere was obtained after the core template was eroded by sodium hydroxide. The wall thickness of the mesoporous cobalt hydroxide hollow sphere could be controlled by changing the reaction time. XRD analysis demonstrated that cobalt (II) hydroxide existed as amorphous. Based on the low-angle X-ray diffraction results, it was concluded that the cobalt hydroxide hollow sphere had mesoscopic structure. XPS spectra shows the characteristic Co 2p peaks at 798.37 and 782.47eV with the separation of 15.9eV between Co 2p_(1/2) and Co 2p_(3/2), which confirmed that Co mainly existed as Co(OH)_2. The formation of the mesoporous cobalt hydroxide shell has been further confirmed by the nitrogen adsorption-desorption experiment. The BET surface area of the hollow sphere (wall thickness: 10nm) is 418m~2/g, and BJH analysis shows that the most probable pore sizes is ca.3.9 nm with narrow size distribution. The thicker the wall thickness is, the smaller the BET surface area of the hollow sphere is. According to the experimental results, the formation mechanism of the nanocomposites with a silica core and a cobalt hydroxide shell was proposed, which is based on the electrostatic attraction between negatively charged silica particles, the positively charged cobalt ions, and the formation of cobalt hydroxide nanotubes was proposed. Firstly, the cobalt hydroxide nanoparticles were formed by hydrolysis of cobalt ions, then, the cobalt hydroxide nanosheets were formed by aggregation of nanoparticles, finally, the cobalt hydroxide nanosheets curled to form nanotubes. Electrochemical test results showed that the hollow sphere of cobalt hydroxide electrode materials demonstrated a higher capacitance and cycle stability than the corresponding bulk cobalt hydroxide. This is due to the larger specific surface area and shorter ion transmission distance of the mesoporous cobalt hydroxide hollow sphere.
3. Synthesis and Characterization of CoFe_2O_4 hollow spheres
Firstly, the micron carbon sphere was formed through the decomposition of glucose during the hydrothermal reaction in the glucose-cobalt sulphate-ammonium ferrous sulfate system. Due to many hydroxyl groups on the surface of carbon sphere, Fe~(2+) , Co~(2+) were directly adsorbed on the carbon sphere surface, as a result, carbon/metal salt core-shell composite was formed. After calcination, the cobalt ferrite hollow sphere could be obtained. EDS and XRD characterization demonstrated that the product was spinel cobalt ferrite. Based on the results of TEM and HRTEM observation, the Size of cobalt ferrite hollow spheres was between 600nm and 900nm, which was formed by the nanocrystalline aggregates with the size of ca.28 nm. Magnetic Properties showed that cobalt ferrite hollow spheres were ferromagnetic. The saturation magnetization of CoFe_2O_4 hollow sphere was 54 emu/g, which was less than that of the bulk cobalt ferrite (72 emu/g). This is due to the nanocrystalline's surface and size effects. The coercivity of CoFe_2O_4 hollow spheres was 860 Oe, and remanence magnetization was 18 emu/g. This material has high saturation magnetization and coercivity. Such material with hydrophilic surface is biocompatible and has potential applications in drug delivery.
1．介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物的合成与表征
利用文献报道的方法，首先制备了四氧化三钴纳米颗粒。然后，将四氧化三钴纳米颗粒分散在一定比例的乙醇-水-氨水-CTAB混合溶液中，加入前驱体TEOS，二氧化硅沉积在四氧化三钴超晶格颗粒的表面，形成介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物。根据广角XRD表征结果，在形成核壳结构复合物的过程中，四氧化三钴物的相未发生变化，表明四氧化三钴具有良好的化学稳定性和水热稳定性。低角度XRD表征结果表明，四氧化三钴和二氧化硅具有介观结构。通过改变前驱体TEOS的浓度，可以调节二氧化硅壳层的厚度(10-35nm)。电镜观察表明二氧化硅壳层的存在有效地抑制了高温下Co_3O_4纳米晶的生长。氮气吸附脱附测试结果表明介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物(壳层厚度：20nm)的比表面积为238.6m~2／g，其孔径呈现双模式介孔分布，最可几孔径尺寸分别为2.0nm和8.8nm。随着壳层厚度的增加，核壳纳米结构复合物的比表面积变大。用氢氟酸刻蚀介孔Co_3O_4／介孔SiO_2核壳结构纳米复合物，可以除去二氧化硅壳层，得到介孔四氧化三钴纳米颗粒。氮气吸附测试结果显示介孔四氧化钴的比表面积为86.4m~2／g，最可几孔径尺寸是8.7nm。实验结果证明核壳结构复合物的形成是源于荷负电的Co_3O_4纳米颗粒、荷正电的CTAB胶束、荷负电的水解聚硅酸根之间的静电引力。这为核壳结构复合物的合成及由纳米晶聚集形成的介孔材料的合成提供了一条新的路线。电化学测试结果表明，与未包覆的四氧化钴纳米颗粒相比，介孔Co_3O_4／介孔SiO_2核壳纳米结构复合物显示出更高的放电容量，这是由于二氧化硅壳层抑制Co_3O_4纳米晶生长，导致复合物具有尺寸更小的Co_3O_4纳米晶的缘故。
2．介孔氢氧化亚钴纳米空心球的合成与表征
首先，采用文献报道的方法合成出二氧化硅纳米颗粒，颗粒尺寸约为75nm。然后，将一定量的二氧化硅纳米颗粒分散于去离子水中，分别加入一定比例的尿素、硝酸钴，在80℃进行回流，氢氧化亚钴沉积在二氧化硅纳米颗粒的表面，得到二氧化硅／介孔氢氧化亚钴核壳结构纳米复合物。用氢氧化钠溶液刻蚀二氧化硅／介孔氢氧化亚钴核壳纳米结构复合物，除去二氧化硅模板，得到介孔氢氧化亚钴空心球。通过改变反应时间，可以实现对介孔氢氧化亚钴纳米空心球壁层厚度的控制(10-25nm)。XRD表征表明氢氧化亚钴为无定形态。用0.5M的氢氧化钠溶解复合物中的二氧化硅，得到氢氧化亚钴纳米空心球。相应的低角度XRD谱图在2θ≈1.5°出现一宽的衍射峰，表明氢氧化亚钴空心球具有无序介孔结构，电镜观察表明介孔是由氢氧化亚钴纳米管而导致，这是首次利用液相技术制备具有均匀内直径的氢氧化亚钴纳米管。根据XPS表征结果，在复合物中，Co 2p的特征峰位于798.37eV和782.47eV，Co 2p_(1／2)和Co 2p_(3／2)的电子结合能间隔为15.9eV，证明复合物中钴是以氢氧化亚钴形式存在。根据氮气吸附测试的结果，氢氧化亚钴空心球(壁层厚度：10nm)的比表面积为418m~2／g，其最可几孔径尺寸为3.9nm，孔径尺寸的分布范围相对较窄。随着壁层厚度的增加，氢氧化亚钴空心球的比表面积减小。实验结果证明核壳结构复合物的形成是源于荷负电的二氧化硅纳米颗粒、荷正电的水合钴离子之间的静电引力，而氢氧化亚钴纳米管的形成则经历了氢氧化亚钴纳米颗粒——氢氧化亚钴纳米片层——氢氧化亚钴纳米管的变化过程。电化学测试结果表明，与块体氢氧化亚钴相比，该氢氧化亚钴纳米空心球电极材料显示出更高的比电容和循环稳定性，这是由于氢氧化亚钴纳米空心球具有更大的比表面积和较短的离子传输距离的缘故。
3．铁酸钴空心球的合成与表征
将葡萄糖-硫酸钴-硫酸亚铁铵的混合溶液进行水热处理，葡萄糖首先通过水热反应，形成微米级碳球。碳球的表面具有许多羟基，混合溶液中的Fe~(2+)、Co~(2+)能够直接吸附在碳球的表面，形成碳球／金属盐核壳结构复合物。通过焙烧处理除去碳球，得到铁酸钴空心球。XRD和EDS表征结果证实产物是铁酸钴。TEM和HRTEM观测的结果表明铁酸钴空心球的尺寸介于600nm-900nm之间，壁层厚度约为150nm。铁酸钴空心球由纳米晶聚集而成，纳米晶的尺寸约为28nm。磁性质测试结果表明，铁酸钴空心球具有铁磁性。其饱和磁化强度为54emu／g，小于块体铁酸钴的饱和磁化强度(72emu／g)。这是由于铁酸钴空心球为纳米晶聚集体，具有表面效应和小颗粒尺寸效应的缘故。铁酸钴空心球的矫顽力为860Oe，剩余磁化强度是18emu／g。该材料具有较高的磁饱和强度和矫顽力。这种表面亲水的材料具有生物相容性，在药物传输方面具有潜在的应用价值。
In this paper, the core-shell nanostructures were prepared using simple liquid chemical methods (sol-gel method; homogeneous precipitation method; hydrothermal method). On the basis of this composite, the hollow sphere was obtained after the core template was removed by chemical etching or calcination. The shell thickness could be controlled by changing the concentration of precursor or reaction time. Based on the experiment, the formation mechanisms of core-shell structure and the mesopores were studied. It was discussed how the structure has effect on its electrochemical properties or magnetic properties.
1. Fabrication and Characterization of Mesoporous Co_3O_4 Core/MesoporousSilica Shell Nanocomposites
The parent Co_3O_4 particles comprised of oriented-aggregated nanocrystals was firstly prepared followed our previous report. Then, the Co_3O_4 nanoparticles were dispersed in a certain proportion of ethanol-water-ammonia-CTAB mixture. After the addition of the precursor TEOS, the silica directly deposited on the surface of Co_3O_4 nanoparticles, and the mesoporous Co_3O_4/mesoporous silica core/shell nanocomposite was formed. Based on the wide-angle X-ray diffraction results, both of the bare Co_3O_4 nanoparticles and the coated Co_3O_4 nanoparticles exhibit the same spinel structure. So it is concluded that Co_3O_4 nanoparticles has good chemical stability and thermal stability. Based on the low-angle X-ray diffraction results, it is confirmed that the Co_3O_4 core and the silica shell have mesostructures. TEM observation indicates that the presence of the silica shell effectively prevents the Co_3O_4 nanocrystals from growing. The thickness of silica shell could be controlled by changing the concentration of precursor TEOS. Based on the experiments, the formation mechanism of the nanocomposite with a mesoporous silica shell and a mesoporous Co_3O_4 core was proposed, which is based on the electrostatic attraction between negatively charged parent Co_3O_4 particles, the positively charged CTAB micelles and the negatively charged silicate species. The mesoporous structure of the Co_3O_4 core and the silica shell has been further confirmed by the N_2 adsorption-desorption isotherm. This work might provide a novel route to core/shell nanostructures and the mesoporous materials from the aggregating of the nanocrystals. Electrochemical analysis reveals that the composite shows a relatively higher discharge capacity comparing to its corresponding bare Co_3O_4 nanoparticles.
2. Synthesis and Characterization of Mesoporous cobalt hydroxide nano-hollow sphere
Firstly, the silica nanoparticles were synthesized according to previous report. The average size of silica particles is about 75 nm. Then, a certain amount of silica nanoparticles were dispersed in deionized water. After the addition of the urea and cobalt nitrate, the solution was heated to 80℃, and refluxed at that temperature for 2 hours. As a result, the cobalt (II) hydroxide was deposited on the surface of silica, and the silica core/mesoporous cobalt (II) hydroxide shell nanocomposite was formed. On the basis of the nanocomposite, the mesoporous cobalt (II) hydroxide hollow sphere was obtained after the core template was eroded by sodium hydroxide. The wall thickness of the mesoporous cobalt hydroxide hollow sphere could be controlled by changing the reaction time. XRD analysis demonstrated that cobalt (II) hydroxide existed as amorphous. Based on the low-angle X-ray diffraction results, it was concluded that the cobalt hydroxide hollow sphere had mesoscopic structure. XPS spectra shows the characteristic Co 2p peaks at 798.37 and 782.47eV with the separation of 15.9eV between Co 2p_(1/2) and Co 2p_(3/2), which confirmed that Co mainly existed as Co(OH)_2. The formation of the mesoporous cobalt hydroxide shell has been further confirmed by the nitrogen adsorption-desorption experiment. The BET surface area of the hollow sphere (wall thickness: 10nm) is 418m~2/g, and BJH analysis shows that the most probable pore sizes is ca.3.9 nm with narrow size distribution. The thicker the wall thickness is, the smaller the BET surface area of the hollow sphere is. According to the experimental results, the formation mechanism of the nanocomposites with a silica core and a cobalt hydroxide shell was proposed, which is based on the electrostatic attraction between negatively charged silica particles, the positively charged cobalt ions, and the formation of cobalt hydroxide nanotubes was proposed. Firstly, the cobalt hydroxide nanoparticles were formed by hydrolysis of cobalt ions, then, the cobalt hydroxide nanosheets were formed by aggregation of nanoparticles, finally, the cobalt hydroxide nanosheets curled to form nanotubes. Electrochemical test results showed that the hollow sphere of cobalt hydroxide electrode materials demonstrated a higher capacitance and cycle stability than the corresponding bulk cobalt hydroxide. This is due to the larger specific surface area and shorter ion transmission distance of the mesoporous cobalt hydroxide hollow sphere.
3. Synthesis and Characterization of CoFe_2O_4 hollow spheres
Firstly, the micron carbon sphere was formed through the decomposition of glucose during the hydrothermal reaction in the glucose-cobalt sulphate-ammonium ferrous sulfate system. Due to many hydroxyl groups on the surface of carbon sphere, Fe~(2+) , Co~(2+) were directly adsorbed on the carbon sphere surface, as a result, carbon/metal salt core-shell composite was formed. After calcination, the cobalt ferrite hollow sphere could be obtained. EDS and XRD characterization demonstrated that the product was spinel cobalt ferrite. Based on the results of TEM and HRTEM observation, the Size of cobalt ferrite hollow spheres was between 600nm and 900nm, which was formed by the nanocrystalline aggregates with the size of ca.28 nm. Magnetic Properties showed that cobalt ferrite hollow spheres were ferromagnetic. The saturation magnetization of CoFe_2O_4 hollow sphere was 54 emu/g, which was less than that of the bulk cobalt ferrite (72 emu/g). This is due to the nanocrystalline's surface and size effects. The coercivity of CoFe_2O_4 hollow spheres was 860 Oe, and remanence magnetization was 18 emu/g. This material has high saturation magnetization and coercivity. Such material with hydrophilic surface is biocompatible and has potential applications in drug delivery.
引文
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