CN105521809B - 一种Cu:ZnO/N:rGO复合光催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种Cu掺杂ZnO纳米棒和N掺杂还原氧化石墨烯(rGO)构成的p‑n结型Cu:ZnO/N:rGO复合光催化剂的制备方法，该催化剂由N掺杂的n型rGO包覆Cu掺杂的p型ZnO纳米棒组成。其制备方法如下：先利用水热法制备Cu掺杂的ZnO纳米棒，然后将其和氧化石墨烯(GO)利用水热还原法组装在一起形成Cu:ZnO/rGO复合光催化剂，最后对Cu:ZnO/rGO在NH3气氛下退火处理进行掺N得到Cu:ZnO/N:rGO复合光催化剂。此方法制备的光催化剂在紫外光下具有很高的光催化活性，且能抑制ZnO的光腐蚀现象，使催化剂的稳定性大大提高，在污水处理领域有重要的潜在应用价值。
Description
技术领域
本发明涉及一种光催化剂的制备方法，属于半导体纳米光催化材料技术领域。
背景技术
能源短缺与环境污染问题是人类未来将要面临的最主要挑战，而光催化分解水及降解污染物被认为是解决这两个问题的有效方法。相比传统的TiO2，同为宽禁带半导体的ZnO拥有更丰富的来源和更高的量子效率，被认为是有潜力替代TiO2的材料之一。ZnO是一种原材料丰富，环境友好的半导体材料，带隙宽(Eg≈3.3eV)，在紫外光照射下能够产生具有很强氧化还原能力的空穴和电子。因此，ZnO理论上具有与TiO2相近的光催化能力。然而，由于光生载流子的迅速复合导致ZnO光催化性能降低和光腐蚀造成的自身结构不稳定，这两个问题严重制约了ZnO在光催化领域的发展。
将石墨烯与ZnO进行复合制备ZnO/rGO复合光催化剂是一种有效提高ZnO光催化性能和光腐蚀抗性的方法。现有技术中尚未见对ZnO和rGO同时进行掺杂后再复合的研究和报道。本发明通过Cu掺杂制备出p型ZnO，然后与N掺杂的n型rGO复合形成纳米p-n结型复合光催化剂，利用rGO优良的电子传递性能和p-n结存在的内建电场抑制光生载流子的复合，有效提高光催化性能。
发明内容
本发明的目的是提供一种制备成本低、工艺简单的Cu:ZnO/N:rGO复合光催化剂的制备方法。
本发明的Cu:ZnO/N:rGO复合光催化剂，由Cu掺杂的ZnO纳米棒和包覆于上述纳米棒外的N掺杂还原氧化石墨烯(rGO)构成。制备方法包括以下步骤：
1)将Zn(CH3COOH)2·2H2O、HMTA和Cu(CH3COO)2溶于去离子水中，使Zn(CH3COOH)2·2H2O和HMTA的浓度均为30mM，Cu(CH3COO)2浓度为0.3mM～0.9mM，获得混合溶液，将混合溶液置于反应釜中在90℃下保温4h，将得到的沉淀物离心洗净并干燥，获得Cu掺杂的ZnO纳米棒；
2)将步骤1)的Cu掺杂ZnO纳米棒分散在去离子水中，然后加入5wt％的GO溶液，充分搅拌1h后，转移至水热釜中120℃水热保温12h，将得到的沉淀物离心洗净并干燥，获得Cu:ZnO/rGO粉末；
3)将步骤2)的Cu:ZnO/rGO粉末置于石英舟中，先通5min NH3和Ar混合气，其中NH3体积含量为10％，然后以20℃/min的速度升温至200℃，随即在5min内匀速升温至300℃～500℃后随炉降温至室温，取出样品得到Cu:ZnO/N:rGO复合光催化剂。
本发明的Cu:ZnO/N:rGO复合光催化剂提升ZnO光催化性能和光腐蚀抗性的原理是：Cu掺杂使本征n型ZnO变为p型，与N掺杂的rGO复合后比表面积增大，光催化反应活性位点增多，反应速率增大；其次p型ZnO与n型rGO形成纳米级别的p-n结，由于内建电场的存在，光生载流子能够迅速地从ZnO转移至N:rGO上，抑制了光生载流子的复合，使光催化性能提高。提高光腐蚀抗性的原因主要有：rGO与ZnO之间C-O的强烈杂化作用能够有效抑制ZnO表面O原子的活性，增强ZnO的稳定性；包覆在ZnO表面的rGO起到类似壁垒的作用，防止ZnO因光腐蚀而结构被破坏；rGO巨大的比表面积能够吸附染料分子，而染料分子能够捕获空穴，与导致ZnO光腐蚀的反应形成竞争，降低了ZnO光腐蚀程度。
本发明的有益效果在于：
1)本发明Cu:ZnO/N:rGO复合光催化剂制备方法简单，可重复性好，产率较高，制备出的复合光催化剂结构稳定，性能优良。
2)Cu:ZnO/N:rGO复合光催化剂对常见污染物有很高的光催化降解活性，而且比常见的未掺杂ZnO-rGO光催化剂的性能更好，能够在更短的时间内完成对污水的光催化净化。
3)本发明的Cu:ZnO/N:rGO复合光催化剂具有优秀的光腐蚀抗性，经过多次光催化循环降解实验后仍能保持较高的光催化活性。
附图说明
图1为Cu:ZnO/N:rGO的XRD衍射图片。
图2为Cu:ZnO/N:rGO的SEM图片。
图3为Cu:ZnO/N:rGO的TEM图片。
图4为Cu:ZnO/N:rGO的Mott-Schottky曲线。
图5为Cu:ZnO/N:rGO和ZnO的N2吸附脱附曲线。
图6为Cu:ZnO/N:rGO、ZnO-rGO和ZnO的光催化降解RhB性能对比图，其中纵坐标C/C0表示剩余浓度与初始浓度的比值。
图7为Cu:ZnO/N:rGO和ZnO的循环光催化降解RhB测试。
具体实施方式
实施例1
(1)将0.659g Zn(CH3COOH)2·2H2O、0.42g HMTA、6mg Cu(CH3COO)2·2H2O加入到100ml去离子水中，持续搅拌至充分溶解，取70ml混合溶液置于100ml反应釜中在90℃下保温4h，将得到的沉淀物离心洗净并干燥获得Cu掺杂的ZnO纳米棒；
(2)将步骤(1)所制备的Cu掺杂ZnO纳米棒分散在去离子水中，然后加入5wt％的GO溶液，充分搅拌1h后将混合溶液转移至水热釜中120℃水热保温12h，然后将得到的沉淀物离心洗净并干燥获得Cu:ZnO/rGO粉末。
(3)所步骤(2)制备的Cu:ZnO/rGO粉末置于石英舟中，先通5min NH3体积含量为10％的NH3和Ar混合气，然后以20℃/min的速度升温至200℃，随即在5min内匀速升温至500℃，然后随炉降温至室温，取出样品得到Cu:ZnO/N:rGO复合光催化剂。
图1为Cu:ZnO/N:rGO的XRD衍射图谱，ZnO的衍射峰与标准图谱匹配，由于rGO含量很少，未出现明显的rGO衍射峰。
图2为Cu:ZnO/N:rGO的SEM图片，可清晰地看出ZnO纳米棒直径约为50nm，长度为1μm至几μm，且rGO很好地包覆在ZnO纳米棒表面。
图3为Cu:ZnO/N:rGO的TEM图片，图中看出ZnO纳米棒是沿[001]晶向生长，rGO均匀地包覆着ZnO纳米棒。
图4为Cu:ZnO/N:rGO的Mott-Schottky曲线，典型的倒“V”型曲线表明形成了p-n结结构。
图5为Cu:ZnO/N:rGO和ZnO的N2吸附脱附曲线，从曲线中可看出Cu:ZnO/N:rGO复合光催化剂比表面积比ZnO大大提高。
图6为Cu:ZnO/N:rGO、ZnO-rGO和ZnO的光催化性能对比图，表明p-n结结构的Cu:ZnO/N:rGO复合光催化剂拥有更好的光催化性能。
图7为Cu:ZnO/N:rGO和ZnO的循环光催化降解实验，说明Cu:ZnO/N:rGO复合光催化剂的光腐蚀抗性明显提高。
实施例2
(1)将0.659g Zn(CH3COOH)2·2H2O、0.42g HMTA、12mg Cu(CH3COO)2·2H2O加入到100ml去离子水中，持续搅拌至充分溶解，取70ml混合溶液置于100ml反应釜中在90℃下保温4h，将得到的沉淀物离心洗净并干燥获得Cu掺杂的ZnO纳米棒；
(2)将步骤(1)所制备的Cu掺杂ZnO纳米棒分散在去离子水中，然后加入5wt％的GO溶液，充分搅拌1h后将混合溶液转移至水热釜中120℃水热保温12h，然后将得到的沉淀物离心洗净并干燥获得Cu:ZnO/rGO粉末。
(3)将步骤(2)所制备的Cu:ZnO/rGO粉末置于石英舟中，先通5min NH3体积含量为10％的NH3和Ar混合气，然后以20℃/min的速度升温至200℃，随即在5min内匀速升温至300℃，然后随炉降温至室温，取出样品得到Cu:ZnO/N:rGO复合光催化剂。
实施例3
(1)将0.659g Zn(CH3COOH)2·2H2O、0.42g HMTA、18mg Cu(CH3COO)2·2H2O加入到100ml去离子水中，持续搅拌至充分溶解，取70ml混合溶液置于100ml反应釜中在90℃下保温4h，将得到的沉淀物离心洗净并干燥获得Cu掺杂的ZnO纳米棒；
(2)将步骤(1)所制备的Cu掺杂ZnO纳米棒分散在去离子水中，然后加入5wt％的GO溶液，充分搅拌1h后将混合溶液转移至水热釜中120℃水热保温12h，然后将得到的沉淀物离心洗净并干燥获得Cu:ZnO/rGO粉末。
(3)将步骤(2)所制备的Cu:ZnO/rGO粉末置于石英舟中，先通5min NH3体积含量为10％的NH3和Ar混合气，然后以20℃/min的速度升温至200℃，随即在5min内匀速升温至400℃，然后随炉降温至室温，取出样品得到Cu:ZnO/N:rGO复合光催化剂。
Claims (1)
1.一种Cu:ZnO/N:rGO复合光催化剂的制备方法，该复合光催化剂由Cu掺杂的ZnO纳米棒和包覆在上述纳米棒外的N掺杂rGO构成，其特征在于，该复合光催化剂的制备方法包括以下步骤：
1)将Zn(CH3COOH)2·2H2O、HMTA和Cu(CH3COO)2溶于去离子水中，使Zn(CH3COOH)2·2H2O和HMTA的浓度均为30mM，Cu(CH3COO)2浓度为0.3mM～0.9mM，获得混合溶液，将混合溶液置于反应釜中在90℃下保温4h，将得到的沉淀物离心洗净并干燥，获得Cu掺杂的ZnO纳米棒；
2)将步骤1)的Cu掺杂ZnO纳米棒分散在去离子水中，然后加入5wt％的GO溶液，充分搅拌1h后，转移至水热釜中120℃水热保温12h，将得到的沉淀物离心洗净并干燥，获得Cu:ZnO/rGO粉末；
3)将步骤2)的Cu:ZnO/rGO粉末置于石英舟中，先通5min NH3和Ar混合气，其中NH3体积含量为10％，然后以20℃/min的速度升温至200℃，随即在5min内匀速升温至300℃～500℃后随炉降温至室温，取出样品得到Cu:ZnO/N:rGO复合光催化剂。
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| CN109402703A (zh) * | 2018-10-08 | 2019-03-01 | 太原理工大学 | 一种耐光腐蚀的二氧化钛/硒化镉/石墨烯薄膜的制备方法 |
| CN110052272B (zh) * | 2019-04-23 | 2020-10-27 | 北京化工大学 | Co掺杂ZnO纳米花材料的制备方法及其应用 |
| CN110813293A (zh) * | 2019-10-31 | 2020-02-21 | 曲阜师范大学 | Cu NPs-rGO电催化剂的制备方法及其应用 |
| CN112619642A (zh) * | 2020-12-18 | 2021-04-09 | 江苏懂醛检测技术有限公司 | 一种微光反应氧催媒石墨烯材料及基于其的空气治理系统 |
| CN113061421B (zh) * | 2021-03-25 | 2022-04-12 | 西北工业大学 | 一种ZnO/N掺杂的中空介电型吸波材料及其制备方法和应用 |
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