新型光催化材料的制备及其可见光催化制氢或制氧性能研究
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摘要
探索高效、稳定和经济的可见光催化材料是光催化制氢技术实用化的关键之一。WO3和BiVO4是为数不多的可见光催化产氧材料,而可控合成具有独特微观形貌、晶相和光吸收性能的WO3和BiVO4及其对产氧效率的影响的研究并不多见。窄带隙(2.4 eV)的CdS具有优异的可见光催化产氢活性,但易发生光腐蚀限制了其应用。将CdS与异质基体复合能抑制光催化过程中的CdS的团聚和光腐蚀。纤维素和多壁碳纳米管均为CdS潜在的支撑体,但是迄今为止尚未见有相关的文献报道。为此,本论文开展了具有特殊微观形貌的BiVO4和WO3,CdS／纤维素复合膜和CdS/MWCNT复合材料的合成研究,深入探讨了反应条件、复合比例等对产物的微观形貌、晶相组成、光吸收和光催化性能的影响,初步揭示了光催化材料具有较高的催化活性和光稳定性的内在原因。采用电化学手段对BiVO4膜电极的光电化学行为、膜内电子输运与复合的影响进行了较为系统的研究。主要研究内容和结论归纳如下：
(1)均相沉淀法制备了具有优异的可见光吸收能力的准球状单斜晶系纳米BiVO4,粒径分布范围19.4-38.9 nm。对比研究了BiVO4／AgNO3和BiVO4／Fe(NO3)3悬浮体系的光催化产氧性能及其长效稳定性。发现,BiVO4／AgNO3体系中光还原所形成的单质Ag负载在BiVO4表面,利于光生载流子的有效分离,可提高体系的产氧效率,但长时间光照后,过量的Ag负载导致体系的稳定性欠佳和再生困难；虽然BiVO4／Fe(NO3)3体系的产氧效率略低,但具有优异的长效稳定性和简便再生性,因而具有更为广阔的实际应用前景。
(2)调节水热反应条件选择性地合成了微球和微片状BiVO4。水热温度较低时(≤160℃)获得产物为由纳米颗粒和纳米片组成的微球状团聚体,团聚体大小在7.12μm之间,为大量BiVO4(z-t)和少量BiVO4(s-m)的混合晶相。当水热温度较高时(200℃)产物是纯相BiVO4(s-m)微米片,厚度在80-120nm之间。较低水热温度下产物倾向形成高对称性BiVO4(z-t)微球,而高温下则易形成不对称结构BiVO4(s-m)微片。光催化实验结果表明,纯相BiVO4(s-m)的产氧效率明显高于混合晶相的产氧效率
(3)以Na2SO4为导向剂水热法合成了六方相WO3纳米棒,并提出了棒状结构的形成机理。0.25M的Na2SO4存在时产物为分散性良好,大长径比的WO3纳米棒,直径在30.150nm之间,长度为0.5-5μm。Na2SO4浓度较小(≤0.25M),水热环境下形成WO3晶种的(200)晶面能大量吸附Na+,致使(001)界面生长形成纳米棒。Na2SO4浓度较大时(≥0.50M),前躯体吸附的Na+浓度过大,不利于立方相H2W2O7脱水晶化为WO3,致使产物为含有立方相H2W2O7和六方相WO3的团聚体。光催化结果显示,分散性良好,大长径比的WO3纳米棒具有最佳的光催化产氧活性。
(4)采用原位沉淀制备了CdS／纤维素(RC)复合膜,通过调节纤维素浓度可调节CdS的固载量。当纤维素浓度从4%增加到5%时,立方相CdS固载量由1.96wt%增加到3.27 wt%,粒径约为8 nm。虽然复合膜中CdS含量小,但由于CdS与纤维素膜有较强相互作用,CdS／RC复合膜显示出优异的可见光催化产氢活性(1.323 mmol g-1h-1)。这主要是因为复合膜中CdS载流子有较快迁移速度,以及CdS粒子与溶液能够有效接触所致。经历10h光照的复合膜的产氢效率仍为5h光照膜效率的93%,说明复合膜具有优良的长效稳定性。此外,复合膜再生极为简便,因而具有极大的应用前景。
(5)将原位吸附与水热法结合制备了CdS／多壁碳纳米管(MWCNT)纳米复合材料。研究了复合比例对复合材料的晶相组成、微观结构和光吸收性能的影响。CNT表面羧基化处理利于复合组分间实现化学键合,发挥协同效应。MWCNT的复合能有效提高材料在可见光吸收范围。与单纯CdS相比,大部分MWCNT/CdS复合材料都表现出更优良的可见光催化产氢活性。长效光照试验中,复合材料光催化产氢量高达2.019 mmol,是单纯CdS产氢量的2.45倍。籍此,认为MWCNT复合提高体系光催化产氢的机理为：CdS吸收可见光后,MWCNT作为电子定向转移通道,降低载流子的复合所致。
(6)采用电化学手段对BiVO4膜电极的光电化学行为、膜内电子输运与复合的影响进行了较为系统的研究。研究了退火温度、膜厚等对电极的瞬态光电流、IPCE及平带电位等的影响。发现：退火温度能显著影响薄膜电极的光电特性。温度低于500℃时,光电活性随着温度的升高而增强,500℃煅烧时达到最大值。此后膜电极内的体相缺陷明显增加,电极的光电活性逐渐降低。IPCE测试结果表明,BiVO4电极有良好的可见光电转换效率,并利用IPCE和hv计算得到BiVO4的带隙为2.36 eV,莫特-肖特基电化学法测得其平带电位为-0.46 V(vs Ag/AgCl)。上述结果为今后BiVO4光催化体系的优化提供了参考依据
Since the photoelelctrochemical splitting of water into H2 and O2 on titaniatitanium oxide (TiO2) electrode was reported in 1972, a great number of attempts on water photosplitting over visible-light responsive semiconductors have been made, with a view to constructing solar energy conversion system to H2 fuel from water in the opinion of the practical application. It is well known that WO3 and BiVO4 is stable and can photo-oxidize water into O2 under visible-light irradiation. Few studies focus on selected-controlled synthesis of WO3 and BiVO4 which are unique morphology, specific crystalline phase, strong light absorption and high activity of photocatalytic O2 evolution. CdS has been extensively studied because of its excellent water photosplitting, property in that its bandgap (ca.2.3 eV). Nevertheless, CdS is prone to photocorrosion during the photochemical reaction because CdS itself is oxidized by the photogenerated holes, which obstructs the large-scale application of the photocatalytic H2 production. Syntheses of CdS nanoparticles in some hetero-matrices have also attracted more research interests as the relative matrix can effectively suppress the photocorrosion of CdS during the photochemical reaction. Cellulose films and multi-walled carbon nanotubes (MWCNT) are quite suitable as host matrixes for the embedment of CdS nano-particles. Though, as far, CdS/MWCNT and CdS/cellulose had not been reported in literature.
Hence, in the present paper, microspheric and lamellar BiV04, nanorods WO3, CdS/MWCNT and CdS/cellulose were prepared. Moreover, the effects of reaction conditions and compound proportion on morphology, crystalline phase, light absorption and photacatalytic activity of the obtained samples were also primarily discussed, which is preliminarily reveals internal cause of high catalytic activity and stability of photocatalyst. The mechanism of photoelectrochemical behavior, electron transfer and recombination of BiVO4 electrodes was systematically studied by electrochemical methods. The detail researches and the conclusions are as follows:
1. Monoclinic BiVO4 nanoparticles were prepared through a homogeneous precipitation process. Photocatalytic O2 evolution efficiencies over the obtained BiVO4 nanoparticles under visible-light (λ> 420nm) irradiation were investigated comparatively by using AgNO3 and Fe(NO3)3 as sacrificial reagent, respectively. It was found that BiVO4/Fe(NO3)3 system is more promising in the opinion of practical application because of long-period photocatalytic activity and conveniently reactivate. However, AgNO3 was a more effective sacrificial reagent for the photocatalytic O2 evolution over the BiVO4 in short-period irradiation in comparison with Fe(NO3)3 attributed to loaded Ag clusters on the surface of BiVO4.
2. Microspheric and lamellar BiVO4 powders were selectively prepared through a hydrothermal process. Microspheric BiV04 of high symmetry with particle sizes in the range of 7-12μm can be derived from a relative low hydrothermal temperature (≤160℃), and possess a mixed crystal consisting of tetragonal and monoclinic phases; whereas dissymmetry lamellar BiVO4 with pure monoclinic phase can be obtained at a higher hydrothermal temperature (200℃). Their photocatalytic activities for O2 evolution were investigated by using Fe(NO3)3 as a sacrificial reagent under visible-light irradiation, and the lamellar BiVO4 shows a better photoactivity than the microspheric product due to its pure monoclinic crystal phase.
3. Nanorods hexagonal WO3 powders were prepared through a simple hydrothermal process by using Na2SO4 as a direction reagent of crystal plane. Nanorods hexagonal WO3 with a diameter of 30-150nm and a length of 0.5μm-5μm can be obtained with 0.25M Na2SO4 at 160℃for 24h. When Na+cation concentration is low (≤0.5M), the coverage of Na+cation at (200) crystal plane of h-WO3 would restrict the further growth of (200) crystal plane, and induce WO3 growth along (001) crystal plane. But once Na+cation concentration is too high (≥1M), Na2SO4 might obstruct the crystal phase transformation from a mixed crystal to pure h-WO3. Their photocatalytic activities for O2 evolution were investigated by using Fe(NO3)3 as a sacrificial reagent under visible-light irradiation, and nanorods hexagonal WO3 shows a high photoactivity due to it's good dispersibility and high length-diameter Ratio.
4. CdS nanoparticles were immobilized in porous regenerated cellulose (RC) films with different pore sizes via in situ a precipitation method. The mean pore sizes of the porous RC films can be modulated from about 20nm to 57 nm by adjusting the concentration of cellulose solution, and the porous structures within RC film act as reacting sites to lead to the embedment of CdS nanoparticles with mean particle diameter of about 8 nm. High photocatalytic H2 production efficiency of about 1.323 mmol g-1 h-1 under visible-light irradiation (λ≥420nm) has been attained over the Pt-loaded CdS/RC nanocomposite film synthesized by 4.5% cellulose solution due to the efficient light absorption, fast carriers transfer and photochemical reaction between the loaded CdS nanoparticles and electrolyte interfaces. In a long-period visible-light irradiation, the present CdS/RC nanocomposite film shows excellent fixity and photostability in comparison with a nanoparticle suspension system, indicating its promising in the practical application, and the present synthesis strategy could be a general method for other semiconductor photocatalyst/porous cellulose films.
5. CdS/MWCNT composites were prepared through in situ adsorption and hydrothermal process. Moreover, the effects of compound proportion on morphology, crystalline phase and light absorption were also discussed. The carboxyls on the surface of CNT would help the achievement of direct chemical bonding between CNT and CdS, which result in synergistic effect of CNT and CdS. MWCNT would contribute to red-shifts in the absorption band for the CdS/MWCNT composites. Compared with CdS, most of CdS/MWCNT composites show higher photocatalytic activity. In a long-period visible-light irradiation, high photocatalytic H2 production efficiency of about 2.019 mmol has been attained over 10% CdS/MWCNT composite, which is 2.4 times higher than that of CdS. A high-energy photon excites an electron from the valence band to the conduction band of CdS photogenerated electrons formed in the space-charge regions are transferred into theMWCNTs, and holes remain on the CdS to take part in redox reactions. This results in the reduced recombination of photogenerated carriers and increase photocatalytic activity of CdS/MWCNT composites.
6. The mechanism of photoelectrochemical behaviors, electron transfer and recombination of BiV04 electrodes was systematically studied by electrochemical methods. The effect of calcination temperature and film thickness of BiVO4 electrodes on the transient photocurrent, monochromatic incident photon-to-electron conversion efficiency and flat-band is also discussed. Calcination temperature can significantly influence the photoelectrochemical characteristics of electrodes. When temperature is low (≤500℃), the photoelectrochemical activity is enhanced with temperature. But once is temperature too high (>500℃), the photoelectrochemical activity is decreased due to the remarked increase of bulk defeats of electrodes. The transient photocurrent spectra show high visible-light photon-to-electron conversion efficiency of BiVO4 electrodes. The band gap of BiVO4 electrodes is 2.36 eV calculated with IPCE and hv. And the flat-band potential (Efb) of semiconductor electrodes measured by Mott-Schottky analysis is-0.46 V (vs Ag/AgCl). The above conclusion is reference of optimization of the BiVO4 photocatalytic system.
(1)均相沉淀法制备了具有优异的可见光吸收能力的准球状单斜晶系纳米BiVO4,粒径分布范围19.4-38.9 nm。对比研究了BiVO4／AgNO3和BiVO4／Fe(NO3)3悬浮体系的光催化产氧性能及其长效稳定性。发现,BiVO4／AgNO3体系中光还原所形成的单质Ag负载在BiVO4表面,利于光生载流子的有效分离,可提高体系的产氧效率,但长时间光照后,过量的Ag负载导致体系的稳定性欠佳和再生困难；虽然BiVO4／Fe(NO3)3体系的产氧效率略低,但具有优异的长效稳定性和简便再生性,因而具有更为广阔的实际应用前景。
(2)调节水热反应条件选择性地合成了微球和微片状BiVO4。水热温度较低时(≤160℃)获得产物为由纳米颗粒和纳米片组成的微球状团聚体,团聚体大小在7.12μm之间,为大量BiVO4(z-t)和少量BiVO4(s-m)的混合晶相。当水热温度较高时(200℃)产物是纯相BiVO4(s-m)微米片,厚度在80-120nm之间。较低水热温度下产物倾向形成高对称性BiVO4(z-t)微球,而高温下则易形成不对称结构BiVO4(s-m)微片。光催化实验结果表明,纯相BiVO4(s-m)的产氧效率明显高于混合晶相的产氧效率
(3)以Na2SO4为导向剂水热法合成了六方相WO3纳米棒,并提出了棒状结构的形成机理。0.25M的Na2SO4存在时产物为分散性良好,大长径比的WO3纳米棒,直径在30.150nm之间,长度为0.5-5μm。Na2SO4浓度较小(≤0.25M),水热环境下形成WO3晶种的(200)晶面能大量吸附Na+,致使(001)界面生长形成纳米棒。Na2SO4浓度较大时(≥0.50M),前躯体吸附的Na+浓度过大,不利于立方相H2W2O7脱水晶化为WO3,致使产物为含有立方相H2W2O7和六方相WO3的团聚体。光催化结果显示,分散性良好,大长径比的WO3纳米棒具有最佳的光催化产氧活性。
(4)采用原位沉淀制备了CdS／纤维素(RC)复合膜,通过调节纤维素浓度可调节CdS的固载量。当纤维素浓度从4%增加到5%时,立方相CdS固载量由1.96wt%增加到3.27 wt%,粒径约为8 nm。虽然复合膜中CdS含量小,但由于CdS与纤维素膜有较强相互作用,CdS／RC复合膜显示出优异的可见光催化产氢活性(1.323 mmol g-1h-1)。这主要是因为复合膜中CdS载流子有较快迁移速度,以及CdS粒子与溶液能够有效接触所致。经历10h光照的复合膜的产氢效率仍为5h光照膜效率的93%,说明复合膜具有优良的长效稳定性。此外,复合膜再生极为简便,因而具有极大的应用前景。
(5)将原位吸附与水热法结合制备了CdS／多壁碳纳米管(MWCNT)纳米复合材料。研究了复合比例对复合材料的晶相组成、微观结构和光吸收性能的影响。CNT表面羧基化处理利于复合组分间实现化学键合,发挥协同效应。MWCNT的复合能有效提高材料在可见光吸收范围。与单纯CdS相比,大部分MWCNT/CdS复合材料都表现出更优良的可见光催化产氢活性。长效光照试验中,复合材料光催化产氢量高达2.019 mmol,是单纯CdS产氢量的2.45倍。籍此,认为MWCNT复合提高体系光催化产氢的机理为：CdS吸收可见光后,MWCNT作为电子定向转移通道,降低载流子的复合所致。
(6)采用电化学手段对BiVO4膜电极的光电化学行为、膜内电子输运与复合的影响进行了较为系统的研究。研究了退火温度、膜厚等对电极的瞬态光电流、IPCE及平带电位等的影响。发现：退火温度能显著影响薄膜电极的光电特性。温度低于500℃时,光电活性随着温度的升高而增强,500℃煅烧时达到最大值。此后膜电极内的体相缺陷明显增加,电极的光电活性逐渐降低。IPCE测试结果表明,BiVO4电极有良好的可见光电转换效率,并利用IPCE和hv计算得到BiVO4的带隙为2.36 eV,莫特-肖特基电化学法测得其平带电位为-0.46 V(vs Ag/AgCl)。上述结果为今后BiVO4光催化体系的优化提供了参考依据
Since the photoelelctrochemical splitting of water into H2 and O2 on titaniatitanium oxide (TiO2) electrode was reported in 1972, a great number of attempts on water photosplitting over visible-light responsive semiconductors have been made, with a view to constructing solar energy conversion system to H2 fuel from water in the opinion of the practical application. It is well known that WO3 and BiVO4 is stable and can photo-oxidize water into O2 under visible-light irradiation. Few studies focus on selected-controlled synthesis of WO3 and BiVO4 which are unique morphology, specific crystalline phase, strong light absorption and high activity of photocatalytic O2 evolution. CdS has been extensively studied because of its excellent water photosplitting, property in that its bandgap (ca.2.3 eV). Nevertheless, CdS is prone to photocorrosion during the photochemical reaction because CdS itself is oxidized by the photogenerated holes, which obstructs the large-scale application of the photocatalytic H2 production. Syntheses of CdS nanoparticles in some hetero-matrices have also attracted more research interests as the relative matrix can effectively suppress the photocorrosion of CdS during the photochemical reaction. Cellulose films and multi-walled carbon nanotubes (MWCNT) are quite suitable as host matrixes for the embedment of CdS nano-particles. Though, as far, CdS/MWCNT and CdS/cellulose had not been reported in literature.
Hence, in the present paper, microspheric and lamellar BiV04, nanorods WO3, CdS/MWCNT and CdS/cellulose were prepared. Moreover, the effects of reaction conditions and compound proportion on morphology, crystalline phase, light absorption and photacatalytic activity of the obtained samples were also primarily discussed, which is preliminarily reveals internal cause of high catalytic activity and stability of photocatalyst. The mechanism of photoelectrochemical behavior, electron transfer and recombination of BiVO4 electrodes was systematically studied by electrochemical methods. The detail researches and the conclusions are as follows:
1. Monoclinic BiVO4 nanoparticles were prepared through a homogeneous precipitation process. Photocatalytic O2 evolution efficiencies over the obtained BiVO4 nanoparticles under visible-light (λ> 420nm) irradiation were investigated comparatively by using AgNO3 and Fe(NO3)3 as sacrificial reagent, respectively. It was found that BiVO4/Fe(NO3)3 system is more promising in the opinion of practical application because of long-period photocatalytic activity and conveniently reactivate. However, AgNO3 was a more effective sacrificial reagent for the photocatalytic O2 evolution over the BiVO4 in short-period irradiation in comparison with Fe(NO3)3 attributed to loaded Ag clusters on the surface of BiVO4.
2. Microspheric and lamellar BiVO4 powders were selectively prepared through a hydrothermal process. Microspheric BiV04 of high symmetry with particle sizes in the range of 7-12μm can be derived from a relative low hydrothermal temperature (≤160℃), and possess a mixed crystal consisting of tetragonal and monoclinic phases; whereas dissymmetry lamellar BiVO4 with pure monoclinic phase can be obtained at a higher hydrothermal temperature (200℃). Their photocatalytic activities for O2 evolution were investigated by using Fe(NO3)3 as a sacrificial reagent under visible-light irradiation, and the lamellar BiVO4 shows a better photoactivity than the microspheric product due to its pure monoclinic crystal phase.
3. Nanorods hexagonal WO3 powders were prepared through a simple hydrothermal process by using Na2SO4 as a direction reagent of crystal plane. Nanorods hexagonal WO3 with a diameter of 30-150nm and a length of 0.5μm-5μm can be obtained with 0.25M Na2SO4 at 160℃for 24h. When Na+cation concentration is low (≤0.5M), the coverage of Na+cation at (200) crystal plane of h-WO3 would restrict the further growth of (200) crystal plane, and induce WO3 growth along (001) crystal plane. But once Na+cation concentration is too high (≥1M), Na2SO4 might obstruct the crystal phase transformation from a mixed crystal to pure h-WO3. Their photocatalytic activities for O2 evolution were investigated by using Fe(NO3)3 as a sacrificial reagent under visible-light irradiation, and nanorods hexagonal WO3 shows a high photoactivity due to it's good dispersibility and high length-diameter Ratio.
4. CdS nanoparticles were immobilized in porous regenerated cellulose (RC) films with different pore sizes via in situ a precipitation method. The mean pore sizes of the porous RC films can be modulated from about 20nm to 57 nm by adjusting the concentration of cellulose solution, and the porous structures within RC film act as reacting sites to lead to the embedment of CdS nanoparticles with mean particle diameter of about 8 nm. High photocatalytic H2 production efficiency of about 1.323 mmol g-1 h-1 under visible-light irradiation (λ≥420nm) has been attained over the Pt-loaded CdS/RC nanocomposite film synthesized by 4.5% cellulose solution due to the efficient light absorption, fast carriers transfer and photochemical reaction between the loaded CdS nanoparticles and electrolyte interfaces. In a long-period visible-light irradiation, the present CdS/RC nanocomposite film shows excellent fixity and photostability in comparison with a nanoparticle suspension system, indicating its promising in the practical application, and the present synthesis strategy could be a general method for other semiconductor photocatalyst/porous cellulose films.
5. CdS/MWCNT composites were prepared through in situ adsorption and hydrothermal process. Moreover, the effects of compound proportion on morphology, crystalline phase and light absorption were also discussed. The carboxyls on the surface of CNT would help the achievement of direct chemical bonding between CNT and CdS, which result in synergistic effect of CNT and CdS. MWCNT would contribute to red-shifts in the absorption band for the CdS/MWCNT composites. Compared with CdS, most of CdS/MWCNT composites show higher photocatalytic activity. In a long-period visible-light irradiation, high photocatalytic H2 production efficiency of about 2.019 mmol has been attained over 10% CdS/MWCNT composite, which is 2.4 times higher than that of CdS. A high-energy photon excites an electron from the valence band to the conduction band of CdS photogenerated electrons formed in the space-charge regions are transferred into theMWCNTs, and holes remain on the CdS to take part in redox reactions. This results in the reduced recombination of photogenerated carriers and increase photocatalytic activity of CdS/MWCNT composites.
6. The mechanism of photoelectrochemical behaviors, electron transfer and recombination of BiV04 electrodes was systematically studied by electrochemical methods. The effect of calcination temperature and film thickness of BiVO4 electrodes on the transient photocurrent, monochromatic incident photon-to-electron conversion efficiency and flat-band is also discussed. Calcination temperature can significantly influence the photoelectrochemical characteristics of electrodes. When temperature is low (≤500℃), the photoelectrochemical activity is enhanced with temperature. But once is temperature too high (>500℃), the photoelectrochemical activity is decreased due to the remarked increase of bulk defeats of electrodes. The transient photocurrent spectra show high visible-light photon-to-electron conversion efficiency of BiVO4 electrodes. The band gap of BiVO4 electrodes is 2.36 eV calculated with IPCE and hv. And the flat-band potential (Efb) of semiconductor electrodes measured by Mott-Schottky analysis is-0.46 V (vs Ag/AgCl). The above conclusion is reference of optimization of the BiVO4 photocatalytic system.
引文
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