不同形貌、不同组分氧化亚铜的制备及其光催化性能研究
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摘要
Ti02和ZnO是目前使用最普遍的半导体光催化剂。然而,这两种材料由于禁带宽度宽,只能被近紫外光和紫外光激活,而紫外光和近紫外光占太阳能总量不到5%。因此,寻找能充分利用太阳能、在可见光范围内具有高活性的光催化剂成为科研工作者近年来探索的主要方向。大约43%的太阳光位于可见光区,只有能够被可见光激发的光催化剂才能充分利用太阳能。Cu20的禁带宽度为2.17eV,可被波长为400-800nm的可见光激发,在太阳光的照射下能有效地产生光生载流子,因此,它有望应用于太阳能转换和可见光催化降解污染物。但是,单相光催化剂由于电子和空穴容易再复合,量子效率非常低,极大地限制了Cu20的开发利用。为了提高Cu20的光催化降解效率,本文先后制备了Cu/Cu2O纳米复合材料和不同形貌的Cu20纳米材料。本文的研究工作主要分为以下3个方面：
1.采用一步液相溶剂热法以硝酸铜((Cu(NO3)2·3H2O)为原料,PVP为保护剂,EG为溶剂、还原剂,成功将Cu2+还原成一价Cu2O。在180℃条件下,通过改变反应时间得到不同形貌、不同组分Cu/Cu2O纳米复合材料,并结合光催化机理讨论了不同组分对复合材料光催化性能的影响。结果表明,随着反应时间的延长,Cu/Cu2O纳米复合材料中Cu的含量逐渐增多,这种组分的变化也引起了复合材料光催化性能的变化。在可见光下辐照20min后,低Cu含量样品(S2-S4：2.1-9.2%)对MO的光催化降解效率分别达到99.78%,99.77%和98.39%。在相同的条件下,与S2-S4相比,纯的Cu20和高Cu含量样品(S5,S6：68%和96%)对MO的光催化降解效率分别只达到了45.88%,73.03%和51.22%。即使在可见光下辐照50min后,降解效率也分别只有85.30%,94.67%和69.33%。此外,我们对Cu/Cu2O纳米复合材料的光催化机理也进行了探讨,并通过周期实验对样品的光稳定性也进行了检测。
2.采用一步液相溶剂热法以Cu(NO3)2·3H2O为原料,PVP为保护剂、表面活性剂,EG为溶剂、还原剂,成功将Cu2+还原成一价Cu2O。通过改变PVP和EG的浓度分析了二者对Cu20纳米材料形貌的影响,并结合光催化机理讨论了二者对Cu20光催化性能的影响。结果表明,固定EG的量,可以通过改变PVP的浓度来控制Cu20纳米材料不同晶面的生长速率,实现形貌可控。当PVP/Cu(NO3)2·3H2O的质量比例为0.022时,得到形貌为球形表面覆盖纳米刺的Cu2O纳米材料,随着PVP/Cu(NO3)2·3H2O的质量比例上升为0.067时,得到形貌为球形表面覆盖方角的Cu20材料,将PVP/Cu(NO3)2·3H2O的质量比例从0.067继续上升为0.111时,得到形貌为球形表面覆盖纳米球形小颗粒的Cu20材料。固定PVP的量,可以通过改变EG的浓度得到形貌为球形表面覆盖纳米刺和纳米球形小颗粒的Cu2O。此外,通过对反应不同时间所制备样品的形貌进行观察发现,本体系所制备的球形Cu20均为空心球,当反应时间为20min时,球形为破裂、开口的空心球,当反应时间为30min时,Cu20生长为完整的球形。不同形貌的Cu20纳米材料,比表面积越大光催化性能越好。在可见光下辐照10min后,Cu20纳米材料(S1-S5)对MO的光降解效率分别达到97.69%,10.36%,42.44%,89.93%和99.67%。通过对比可知,在相同的条件下,形貌为球形表面覆盖纳米刺的Cu20纳米材料(S1,S5)表现出了最佳的光催化活性。
3.采用一步液相溶剂热法以Cu(NO3)2·3H2O为原料,EG为溶剂、还原剂,分别添加PVP、葡萄糖和水合肼,在180℃条件下成功制得形貌为微米级球形表面覆盖花片、20-50nm小颗粒团聚成小球以及线形的Cu20纳米材料,并结合光催化机理讨论了形貌对Cu20光催化性能的影响。在可见光下辐照10min后,在添加PVP、葡萄糖和水合肼条件下制备的Cu20纳米材料对MO的光催化降解效率分别达到97.50%,61.61%和98.76%。
由于高温条件不利于大批量生产,因此,我们在以上的实验基础之上,尝试在常温、无表面添加剂、无有机溶剂的条件下合成Cu20纳米材料。由于葡萄糖和水合肼具有还原性,在30℃强碱条件下,我们利用葡萄糖和水合肼还原Cu(NO3)2·3H2O,成功制得Cu20纳米材料。在该反应体系中,葡萄糖和水合肼不仅作为还原剂,而且作为形貌控制剂,通过影响Cu20不同晶面的生长速率,合成去角八面体和八面体Cu20,并结合光催化机理讨论了形貌对Cu20光催化性能的影响。在可见光下辐照30min,去角八面体和八面体Cu20的光催化降解效率分别为22.36%和11.30%。
本文制备样品所采用的方法均能一次性合成不同形貌的Cu20纳米材料和不同组分的Cu/Cu2O复合材料,制备方法简单易行,且大大降低生产成本。所制得的材料对甲基橙具有很高的光催化降解率,有望在污水处理和空气净化方面获得应用。
TiO2and ZnO are the most commonly used photocatalysts. However, it is a pity that both of them can only be activated by ultraviolet light or near-ultraviolet light because of their broad band gap (3.0-3.2eV), hence only less than5%solar energy can be utilized. Therefore, finding a kind of photocatalysts which can make full use of solar energy and have high photocatalytic activity have been the main research direction. The majority of irradiation (about43%) of sunlight lies in the visible range, and only photocatalysts with corresponding band gap can make full use of the solar energy. Cuprous oxide (Cu2O) has a direct band gap of about2.17eV, can be inspired by the400-800nm visible-light and product electron hole pair under the irradiation of sunlight,which makes it a promising material for solar energy conversion and visible photocatalytic degradation of pollutants. The single phase photocatalysts exhibit very low quantum efficiency because of the easy recombination between photo-electrons and holes, the development and utilization of Cu2O is greatly limited. In order to improve the photocatalytic ability of Cu2O, Cu/Cu2O NCs and different morphology of Cu2O nanocrystals were synthesized. This thesis consists of three following aspects:
1. we synthesized Cu/Cu2O NCs by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, PVP as the protective agent and EG as the solvent and reducing agent. The phase compositions and morphology of Cu/Cu2O NCs are controlled by adjusting the reaction time. The photocatalytic mechanism of Cu/Cu2O NCs are also investigated. It can be concluded that the content of Cu in the final samples could be tuned by controlling the reaction time at180℃. Otherwise the content of Cu in the Cu/Cu2O NCs plays an important role on the photo-catalytic activity. At the first20min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu/Cu2O NCs with low content of Cu (S2-S4:2.1-9.2%) reach up to99.78%,99.77%,98.39%, respectively. Compared with S2-S4, under the same conditions, the maximum degradation efficiency of MO with pure Cu2O (S1),Cu/Cu2O NCs with a high Cu content (S5, S6:68%and96%) are only45.88%,73.03%and51.22%, respectively, even though after visible light irradiation for50min, only the degradation efficiency of85.30%,94.67%and69.33%. Besides, the photostability of Cu/Cu2O NCs was studied by recycles.
2. we synthesized Cu2O nanocrystals by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, PVP as the protective agent and surfactant, EG as the solvent and reducing agent. The morphology of Cu2O nanocrystals was influenced by the PEG concentrations and EG concentrations. The photocatalytic mechanism of Cu2O nanocrystals were also investigated. When the EG concentrations was the same, PVP kinetically controlled the growth rates of different crystalline faces of Cu2O by interacting with these faces through adsorption and desorption. when the radio of PVP/Cu(NO3)2·3H2O was0.022, it can be clearly seen that the surface of the spheres is covered with Cu2O crystal thorn. As the molar radio of PVP/Cu(NO3)2·3H2O increases from0.022to0.067, the surface of the spheres is covered with Cu2O crystal corner. Increasing the radio of PVP/Cu(NO3)2·3H2O from0.067to0.111, the surface of the spheres is made from an assembly of smaller spherical particles. When the composition of EG increases from50ml to90ml (S3), and other experimental conditions are kept the same, the morphology of the surface of the spheres change from Cu2O crystal thorn into spherical particles. When the reaction time increases from20min to30min (S3), and other experimental conditions are kept the same, the morphology of the obtained samples change from "open mouth" or broken hemispheres into perfect spheres without broken. At the first10min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S1-S5) reach up to97.69%,10.36%,42.44%,89.93%and99.67%respectively, the surface of the spheres covered with Cu2O crystal thorn show the optimal photocatalytic activity.
3. we synthesized Cu2O nanocrystals by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, EG as the solvent and reducing agent. The morphology of Cu2O nanocrystals are controlled by adding PVP、 hydrazine hydrate or glucose. The photocatalytic mechanism of Cu2O nanocrystals are also investigated. At the first10min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S1-S3) reach up to97.50%,61.61%and98.76%respectively.
Due to the high temperature adverse to mass production, herein, we put forward a convenient solution-phase method for the synthesis of Cu2O truncated octahedral and octahedral crystals. The Cu2O crystals were selectively synthesized without surfactant and organic solvent at room temperature, with Cu(NO3)2·3H2O and NaOH as starting reactants, and hydrazine hydrate or glucose as the reducer.At the30min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S4, S5)are22.36%and11.30%.
The Cu/Cu2O CNs and different morphology of Cu2O nanocrystals are synthesized by the simple one-pot route.This method, simple and effective, may be helpful for the study on controlled synthesis of other materials. The high photocatalytic activity of Cu/Cu2O CNs and different morphology of Cu2O nanocrystals suggests they are promising materials for processing of waste water.
1.采用一步液相溶剂热法以硝酸铜((Cu(NO3)2·3H2O)为原料,PVP为保护剂,EG为溶剂、还原剂,成功将Cu2+还原成一价Cu2O。在180℃条件下,通过改变反应时间得到不同形貌、不同组分Cu/Cu2O纳米复合材料,并结合光催化机理讨论了不同组分对复合材料光催化性能的影响。结果表明,随着反应时间的延长,Cu/Cu2O纳米复合材料中Cu的含量逐渐增多,这种组分的变化也引起了复合材料光催化性能的变化。在可见光下辐照20min后,低Cu含量样品(S2-S4：2.1-9.2%)对MO的光催化降解效率分别达到99.78%,99.77%和98.39%。在相同的条件下,与S2-S4相比,纯的Cu20和高Cu含量样品(S5,S6：68%和96%)对MO的光催化降解效率分别只达到了45.88%,73.03%和51.22%。即使在可见光下辐照50min后,降解效率也分别只有85.30%,94.67%和69.33%。此外,我们对Cu/Cu2O纳米复合材料的光催化机理也进行了探讨,并通过周期实验对样品的光稳定性也进行了检测。
2.采用一步液相溶剂热法以Cu(NO3)2·3H2O为原料,PVP为保护剂、表面活性剂,EG为溶剂、还原剂,成功将Cu2+还原成一价Cu2O。通过改变PVP和EG的浓度分析了二者对Cu20纳米材料形貌的影响,并结合光催化机理讨论了二者对Cu20光催化性能的影响。结果表明,固定EG的量,可以通过改变PVP的浓度来控制Cu20纳米材料不同晶面的生长速率,实现形貌可控。当PVP/Cu(NO3)2·3H2O的质量比例为0.022时,得到形貌为球形表面覆盖纳米刺的Cu2O纳米材料,随着PVP/Cu(NO3)2·3H2O的质量比例上升为0.067时,得到形貌为球形表面覆盖方角的Cu20材料,将PVP/Cu(NO3)2·3H2O的质量比例从0.067继续上升为0.111时,得到形貌为球形表面覆盖纳米球形小颗粒的Cu20材料。固定PVP的量,可以通过改变EG的浓度得到形貌为球形表面覆盖纳米刺和纳米球形小颗粒的Cu2O。此外,通过对反应不同时间所制备样品的形貌进行观察发现,本体系所制备的球形Cu20均为空心球,当反应时间为20min时,球形为破裂、开口的空心球,当反应时间为30min时,Cu20生长为完整的球形。不同形貌的Cu20纳米材料,比表面积越大光催化性能越好。在可见光下辐照10min后,Cu20纳米材料(S1-S5)对MO的光降解效率分别达到97.69%,10.36%,42.44%,89.93%和99.67%。通过对比可知,在相同的条件下,形貌为球形表面覆盖纳米刺的Cu20纳米材料(S1,S5)表现出了最佳的光催化活性。
3.采用一步液相溶剂热法以Cu(NO3)2·3H2O为原料,EG为溶剂、还原剂,分别添加PVP、葡萄糖和水合肼,在180℃条件下成功制得形貌为微米级球形表面覆盖花片、20-50nm小颗粒团聚成小球以及线形的Cu20纳米材料,并结合光催化机理讨论了形貌对Cu20光催化性能的影响。在可见光下辐照10min后,在添加PVP、葡萄糖和水合肼条件下制备的Cu20纳米材料对MO的光催化降解效率分别达到97.50%,61.61%和98.76%。
由于高温条件不利于大批量生产,因此,我们在以上的实验基础之上,尝试在常温、无表面添加剂、无有机溶剂的条件下合成Cu20纳米材料。由于葡萄糖和水合肼具有还原性,在30℃强碱条件下,我们利用葡萄糖和水合肼还原Cu(NO3)2·3H2O,成功制得Cu20纳米材料。在该反应体系中,葡萄糖和水合肼不仅作为还原剂,而且作为形貌控制剂,通过影响Cu20不同晶面的生长速率,合成去角八面体和八面体Cu20,并结合光催化机理讨论了形貌对Cu20光催化性能的影响。在可见光下辐照30min,去角八面体和八面体Cu20的光催化降解效率分别为22.36%和11.30%。
本文制备样品所采用的方法均能一次性合成不同形貌的Cu20纳米材料和不同组分的Cu/Cu2O复合材料,制备方法简单易行,且大大降低生产成本。所制得的材料对甲基橙具有很高的光催化降解率,有望在污水处理和空气净化方面获得应用。
TiO2and ZnO are the most commonly used photocatalysts. However, it is a pity that both of them can only be activated by ultraviolet light or near-ultraviolet light because of their broad band gap (3.0-3.2eV), hence only less than5%solar energy can be utilized. Therefore, finding a kind of photocatalysts which can make full use of solar energy and have high photocatalytic activity have been the main research direction. The majority of irradiation (about43%) of sunlight lies in the visible range, and only photocatalysts with corresponding band gap can make full use of the solar energy. Cuprous oxide (Cu2O) has a direct band gap of about2.17eV, can be inspired by the400-800nm visible-light and product electron hole pair under the irradiation of sunlight,which makes it a promising material for solar energy conversion and visible photocatalytic degradation of pollutants. The single phase photocatalysts exhibit very low quantum efficiency because of the easy recombination between photo-electrons and holes, the development and utilization of Cu2O is greatly limited. In order to improve the photocatalytic ability of Cu2O, Cu/Cu2O NCs and different morphology of Cu2O nanocrystals were synthesized. This thesis consists of three following aspects:
1. we synthesized Cu/Cu2O NCs by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, PVP as the protective agent and EG as the solvent and reducing agent. The phase compositions and morphology of Cu/Cu2O NCs are controlled by adjusting the reaction time. The photocatalytic mechanism of Cu/Cu2O NCs are also investigated. It can be concluded that the content of Cu in the final samples could be tuned by controlling the reaction time at180℃. Otherwise the content of Cu in the Cu/Cu2O NCs plays an important role on the photo-catalytic activity. At the first20min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu/Cu2O NCs with low content of Cu (S2-S4:2.1-9.2%) reach up to99.78%,99.77%,98.39%, respectively. Compared with S2-S4, under the same conditions, the maximum degradation efficiency of MO with pure Cu2O (S1),Cu/Cu2O NCs with a high Cu content (S5, S6:68%and96%) are only45.88%,73.03%and51.22%, respectively, even though after visible light irradiation for50min, only the degradation efficiency of85.30%,94.67%and69.33%. Besides, the photostability of Cu/Cu2O NCs was studied by recycles.
2. we synthesized Cu2O nanocrystals by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, PVP as the protective agent and surfactant, EG as the solvent and reducing agent. The morphology of Cu2O nanocrystals was influenced by the PEG concentrations and EG concentrations. The photocatalytic mechanism of Cu2O nanocrystals were also investigated. When the EG concentrations was the same, PVP kinetically controlled the growth rates of different crystalline faces of Cu2O by interacting with these faces through adsorption and desorption. when the radio of PVP/Cu(NO3)2·3H2O was0.022, it can be clearly seen that the surface of the spheres is covered with Cu2O crystal thorn. As the molar radio of PVP/Cu(NO3)2·3H2O increases from0.022to0.067, the surface of the spheres is covered with Cu2O crystal corner. Increasing the radio of PVP/Cu(NO3)2·3H2O from0.067to0.111, the surface of the spheres is made from an assembly of smaller spherical particles. When the composition of EG increases from50ml to90ml (S3), and other experimental conditions are kept the same, the morphology of the surface of the spheres change from Cu2O crystal thorn into spherical particles. When the reaction time increases from20min to30min (S3), and other experimental conditions are kept the same, the morphology of the obtained samples change from "open mouth" or broken hemispheres into perfect spheres without broken. At the first10min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S1-S5) reach up to97.69%,10.36%,42.44%,89.93%and99.67%respectively, the surface of the spheres covered with Cu2O crystal thorn show the optimal photocatalytic activity.
3. we synthesized Cu2O nanocrystals by the simple one-pot solution-phase solvent route. In the experiment, we employed Cu(NO3)2·3H2O as the raw material, EG as the solvent and reducing agent. The morphology of Cu2O nanocrystals are controlled by adding PVP、 hydrazine hydrate or glucose. The photocatalytic mechanism of Cu2O nanocrystals are also investigated. At the first10min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S1-S3) reach up to97.50%,61.61%and98.76%respectively.
Due to the high temperature adverse to mass production, herein, we put forward a convenient solution-phase method for the synthesis of Cu2O truncated octahedral and octahedral crystals. The Cu2O crystals were selectively synthesized without surfactant and organic solvent at room temperature, with Cu(NO3)2·3H2O and NaOH as starting reactants, and hydrazine hydrate or glucose as the reducer.At the30min of irradiation, the photodegradation efficiency of MO solution in the presence of Cu2O NCs (S4, S5)are22.36%and11.30%.
The Cu/Cu2O CNs and different morphology of Cu2O nanocrystals are synthesized by the simple one-pot route.This method, simple and effective, may be helpful for the study on controlled synthesis of other materials. The high photocatalytic activity of Cu/Cu2O CNs and different morphology of Cu2O nanocrystals suggests they are promising materials for processing of waste water.
引文
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