CN110639498B - 一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法 - Google Patents
一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种棒状结构石墨烯量子点/氧化铈复合光催化剂,是将CeO2纳米粒子加入石墨烯量子点水溶液中,超声分散均匀后转入反应釜中进行水热反应;反应结束后冷却,离心分离产物,超纯水洗涤,冷冻干燥,即得棒状结构石墨烯量子点/氧化铈复合光催化剂。本发明以CeO2作为光催化剂,GQDs作为光敏化剂,经水热条件得到在CeO2表面包覆了GQDs的棒状复合材料。水热处理的过程中材料外部的GQDs起到了结构导向作用,使复合材料具有优化的有序棒状特殊形貌;另一方面,小尺寸的GQDs在CeO2表面增强了复合材料可见光照射下电子‑空穴的转移寿命,提高了复合光催化剂的光催化能力,在光催化废水处理等领域具有应用前景。
Description
技术领域
本发明涉及一种氧化铈复合光催化剂,尤其涉及一种具有棒状结构石墨烯量子点/氧化铈(GQDs/CeO2)的制备方法,用于有机污染物的光催化降解,属于复合材料领域及光催化应用领域。
背景技术
氧化铈(CeO2)为常用的光催化剂,其晶体属于萤石型面心立方结构(每个Ce4+离子周围有8个O2-离子),其光吸收阈值可达420 nm,高于常用的半导体材料TiO2。虽然CeO2在催化应用中具有自身优势和潜力,但其较宽的带隙导致在实际应用中催化性能表现并不理想。
石墨烯量子点(GQDs)GQDs具有大比表面积、优异的光电性能、良好的分散性及生物相容性,可用于各种材料的制备过程。GQDs优异的光致电子转移特性,良好的可见光吸收性能,拓宽了的可见光光吸收范围,同时可为光催化反应提供更多有效接触界面和活性位点。研究表明,GQD具有协同提高半导体/GQDs光催化剂的光催化活性的作用,即GQDs作为光敏剂最大化光吸收,可用于提高电荷分离效率的电子受体。因此,将CeO2与GQDs结合制备的复合光催化剂GQDs/CeO2具有更高的有机污染物光降解率。
发明内容
本发明的目的提供一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法。
本发明石墨烯量子点/氧化铈复合光催化剂的制备方法,是将氧化铈(CeO2)纳米粒子加入石墨烯量子(GQDs)点水溶液中,超声分散均匀后转入反应釜中进行水热反应;反应结束后冷却,离心分离产物,超纯水洗涤,冷冻干燥,即得棒状结构石墨烯量子点/氧化铈复合光催化剂(GQDs/CeO2)。
所述CeO2纳米粒子的粒径为150~200 nm;GQDs的粒径为5~7nm,且含氮量为3.1~3.15 at%。GQDs的质量为CeO2粒子质量的1.5~9.0%。
所述水热反应是在100~105℃下保持2.5~3 h。
所述离心分离转速为9000~10000 rpm。
所述冷冻干燥是在-50~-55℃下真空干燥10~12h。
下面通过扫描电镜分析、紫外可见吸收光谱、荧光光谱及光催化等测试表征对本发明GQDs/CeO2材料的结构和性能进行分析说明。
1、扫描电镜分析
图1为CeO2纳米粒子(A、B)及棒状GQDs/CeO2复合材料(C、D)在不同放大倍率下的电镜照片。图1显示,低倍率下CeO2纳米粒子更多地无规则团聚在一起,其中含有部分短棒状的结构;高倍率下CeO2纳米微粒是完整的立方萤石相晶体,CeO2纳米粒子因较大的表面能聚集在一起。当CeO2纳米微粒中加入GQDs形成复合材料GQDs/CeO2 时,由于GQDs具有几个纳米的尺度,因而图中并不能直接观察到其存在。另外复合材料GQDs/CeO2的整个宏观形貌相比CeO2发生了转变,由无序堆积变为有序规则的棒状形貌结构,GQDs包覆在CeO2表面,使其表面能发生变化而形貌转变成为图1(D)中的棒状结构。
2、紫外可见吸收光谱
光电转换材料性能的体现和性能的提升主要表现在其对光的响应能力上,其中对可见光的响应是太阳能利用的一个主要方面,也是光电转换材料在应用领域努力的方向。图2(A)为本发明制备的复合材料GQDs/CeO2的漫反射光谱,从图中可以观察到,与纯的CeO2相比,复合材料的吸收边发生了明显的红移,其中CeO2的吸收边为415 nm,GQDs-4.5/CeO2的吸收边为475 nm,这主要是由于GQDs结构中的 π-π共轭结构的作用引起的。复合材料对紫外可见光的吸收边的拓宽,相比原料能够有效增强对可见光的利用,从而提升可见光下复合材料的催化效率。图2(B)表示通过求(ahν)1/2对光电子能(hν)的斜率得到材料的禁带宽度值,相比原料CeO2的禁带宽度值3.1 eV,复合材料的禁带宽度值减小,GQDs-3.0/CeO2、GQDs-4.5/CeO2和GQDs-6.0/CeO2的禁带宽度值分别为2.98、2.42和2.63 eV,这个结果可以判定GQDs对CeO2的带隙值有很大的影响,因此复合材料GQDs-4.5/CeO2具有比纯CeO2更好的可见光响应性。
3、荧光光谱
通过上述扫描电镜图和紫外可见吸收光谱图知道,GQDs是包裹在CeO2的表面,两者之间存在紧密的界面连接;此外,从紫外-可见吸收光谱表征发现复合材料GQDs/CeO2的带隙相较于纯CeO2发生了变化,这些特征都从侧面反映了GQDs上的光生电子很可能会自由移动至CeO2上,而这个转移的过程会使电子和空穴的寿命延长,更多几率的电子和空穴能更有效地体现其性能,增强复合材料的光电性能。根据前人相关方面的研究,要确定电子和空穴这两者之间分离效率的关系,通常采用光致发光光谱来论证。图3为纯CeO2和GQDs/CeO2复合材料在激发波长为320 nm的光致发光光谱。从图3中可以观察到,纯CeO2和复合材料具有相似的光谱特征,但纯CeO2的光致发光强度远高于几种复合材料GQDs/CeO2,这说明GQDs的引入提高了电子和空穴的分离效率。此外,从图3中可看出不同GQDs含量的复合材料的光致发光光谱中,GQDs-4.5/CeO2的峰值强度最低,这也说明复合材料GQDs-4.5/CeO2具有最佳的光生电子-空穴分离效率。
4、GQDs/CeO2复合材料的光催化性能
CeO2以及GQDs/CeO2光催化有机物降解实验:准确配制一定浓度的罗丹明B(RhB)溶液(CRhB=10 mg·L-1),移取50 mL MB溶液于石英反应器中,随后向加入25 mg光催化剂,在黑暗条件下磁力搅拌1 h,使MB分子在催化剂表面和溶液中达到吸附-脱附平衡;然后打开300W的氙灯光源,滤光片滤掉紫外光(λ>400 nm),在冷却水循环条件下使反应体系温度维持在 25 ℃左右。在光催化实验的进程中每隔相同时间取约4 mL的样品于离心试管中,离心分离上清液,用UV-2550型可见分光光度计测定离心液在λmax=554 nm 处的吸光度,并根据反应后清液中RhB的浓度和初始浓度的变化,计算光催化剂对RhB的去除率。图4为复合材料GQDs/CeO2中GQDs所占的质量百分数为1.5wt%,3.0wt%,4.5wt%,6.0wt%,7.5wt%,9.0wt%的GQDs/CeO2光催化效率对比图。由图4所示还可以看出,经过60 min黑暗条件后达到的吸附平衡,此过程中包括CeO2和复合材料GQDs/CeO2对RhB都具有吸附并且吸附量的差异不大,这是由于GQDs尺寸对吸附过程的影响很小。但是在可见光照射下,GQDs的加入增加了花状CeO2表面的活性位点及对有机物的吸附能力,因此相对于单一CeO2,复合材料GQDs/CeO2的光催化强度提升,使得棒状结构GQDs/CeO2表现出更优越的光催化效率。其中GQDs-4.5/CeO2表现出了最强的催化活性,这说明与GQDs的复合量为4.5 wt%时为最佳的复合量,CeO2能最好地和GQDs配合体现最高的催化活性。测试结果:光照180 min后,纯CeO2对于RhB的去除率为21.9%;GQDs-4.5/CeO2对RhB的去除率为94.4%。
综上所述,本发明利用储量丰富、价格低廉的催化剂CeO2为催化原料,以GQDs为光敏化剂,经水热处理后得到了CeO2表面包覆GQDs的GQDs/CeO2复合材料。一方面,水热处理的过程中材料外部的GQDs起到了结构导向作用,使复合材料GQDs/CeO2具有优化的有序棒状特殊形貌;另一方面,小尺寸的GQDs在CeO2表面增强了复合材料可见光照射下电子-空穴的转移寿命,提高了GQDs/CeO2的光催化能力,在光催化废水处理等领域具有应用前景。
附图说明
图1为CeO2及本发明制备的棒状GQDs/CeO2复合材料的扫描电镜图。
图2为CeO2及本发明制备的棒状GQDs/CeO2复合材料的紫外可见吸收光谱图。
图3为本发明制备的棒状GQDs/CeO2复合材料和CeO2的荧光光谱图。
图4为本发明制备的不同GQDs含量的GQDs/CeO2复合材料光催化降解对比图。
具体实施方式
下面通过具体实例对本发明棒状结构GQDs/CeO2复合材料的制备、性能等作进一步说明。
实施例1
GQDs/CeO2复合材料:称取0.1 g CeO2纳米粒子和1.5 mg GQDs(1.5 wt%)分散于20mL水溶液中,超声分散30 min;然后转入反应釜中,加热至100℃保持3 h;冷却,产物离心分离(转速为9000~10000 rpm),超纯水洗涤,-50℃下真空冷冻干燥10 h,得GQDs-1.5/CeO2复合材料。
GQDs-1.5/CeO2复合材料对于RhB的去除率:180 min为79.3%。
实施例 2
GQDs/CeO2复合材料:称取0.1 g CeO2纳米粒子和3.0 mg GQDs(3.0 wt%)分散于20mL水溶液中,超声分散30 min;然后转入反应釜中,加热至100℃保持3 h;冷却,产物离心分离(转速为9000~10000 rpm),超纯水洗涤,-50℃下真空冷冻干燥10 h,得GQDs-3.0/CeO2复合材料。
GQDs-3.0/CeO2复合材料对于RhB的去除率:180 min为93.3%。
实施例3
GQDs/CeO2复合材料:称取0.1 g CeO2纳米粒子和4.5mg GQDs(4.5 wt%)分散于20mL水溶液中,超声分散30 min;然后转入反应釜中,加热至100℃保持3 h;冷却,产物离心分离(转速为9000~10000 rpm),超纯水洗涤,-50℃下真空冷冻干燥10 h,得GQDs-4.5/CeO2复合材料。
GQDs-4.5/CeO2复合材料对于RhB的去除率:180 min为94.4%。
实施例4
GQDs/CeO2复合材料:称取0.1 g CeO2纳米粒子和6.0 mg GQDs(6.0 wt%)分散于20mL水溶液中,超声分散30 min;然后转入反应釜中,加热至100℃保持3 h;冷却,产物离心分离(转速为9000~10000 rpm),超纯水洗涤,-50℃下真空冷冻干燥10 h,得GQDs-6.0/CeO2复合材料。
GQDs-6.0/CeO2复合材料对于RhB的去除率在180 min:时为92.0%。
Claims (3)
1.一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法,是将CeO2纳米粒子加入石墨烯量子点水溶液中,超声分散均匀后转入反应釜中进行水热反应;反应结束后冷却,离心分离产物,超纯水洗涤,冷冻干燥,即得棒状结构石墨烯量子点/氧化铈复合光催化剂;所述CeO2纳米粒子的粒径为150~200 nm,石墨烯量子点的粒径为5~7nm,且含氮量为3.1~3.15 at%;石墨烯量子点的质量为CeO2粒子质量的1.5~9.0%;所述水热反应是在100~105℃下保持2.5~3 h。
2.如权利要求1所述一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法,其特征在于:所述离心分离转速为9000~10000 rpm。
3.如权利要求1所述一种棒状结构石墨烯量子点/氧化铈复合光催化剂的制备方法,其特征在于:所述冷冻干燥是在-50~-55℃下真空干燥10~12h。
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