CN105521809A - 一种Cu:ZnO/N:rGO复合光催化剂的制备方法 - Google Patents
一种Cu:ZnO/N:rGO复合光催化剂的制备方法 Download PDFInfo
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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5minNH3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0.659gZn(CH3COOH)2·2H2O、0.42gHMTA、6mgCu(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5minNH3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0.659gZn(CH3COOH)2·2H2O、0.42gHMTA、12mgCu(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5minNH3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0.659gZn(CH3COOH)2·2H2O、0.42gHMTA、18mgCu(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5minNH3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5minNH3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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CN108321404A (zh) * | 2018-03-01 | 2018-07-24 | 哈尔滨工业大学 | 一种金属或金属氧化物/掺杂型石墨烯核壳型催化剂载体与担载型催化剂及其制备方法 |
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CN113061421A (zh) * | 2021-03-25 | 2021-07-02 | 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 |
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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