CN110586165A - 一种氮掺杂改性的g-C3N4光催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种氮掺杂改性的g‑C3N4光催化剂及其制备方法和应用。将尿素和DMF混合均匀后放入坩埚,然后将坩埚置于马弗炉中煅烧,保温一段时间后放入玛瑙研钵中研磨,即得到CNU‑DMF光催化剂。CNU‑DMF光催化剂可用作在可见光条件下高效光催化裂解水制氢。本发明将DMF用于改性g‑C3N4,与原始g‑C3N4相比,CNU‑DMF光催化剂具有更大的比表面积,光吸收能力显著增强,并且光生电子‑空穴复合率降低,光催化活性得到明显的提高。本发明制备工艺简单、生产成本低、容易操作、原料来源充足,CNU‑DMF光催化剂稳定性高,在实际应用方面有很大的潜力。
Description
技术领域
本发明涉及光催化剂,具体的说是一种氮掺杂改性的g-C3N4光催化剂及其制备方法。
背景技术
随着能源需求和环境问题的日益严峻,人们开始开发绿色可再生资源来替代化石燃料。目前,利用半导体光催化剂光催化裂解水制氢被认为是解决能源危机和环境问题的一种很有前途的方法。TiO2作为一种用于光催化制氢的半导体材料,其自身存在较大缺陷,即大带隙(3.2eV)、低可见光响应以及高的电子-空穴复合速率,导致了光催化活性低,限制了其潜在的应用前景。因此,探索一种高可见光响应并具有良好光催化活性的光催化剂是一项具有重要意义的工作。
在过去几年里,研究人员一直致力于设计和制造高效、稳定和低成本的光催化剂。g-C3N4作为一种具有可见光响应的无金属半导体光催化剂,由于其具有合适的能带结构、物理化学性质稳定、制备方法简单、低成本、对环境无危害等优点,受到了人们的广泛关注。然而,g-C3N4也存在着自身的缺陷,如吸光能力弱、比表面积低、光生电子-空穴复合效率快等,导致光催化活性降低,限制了其实际应用。为了克服这些缺点,人们通过多种方法对g-C3N4进行改性以提高其光催化活性。如物理/化学剥落,金属/非金属掺杂,异质结的制备等。其中,通过非金属掺杂改性g-C3N4由于其经济成本较低,操作简单,是提高g-C3N4光催化活性是一有效策略。
发明内容
为了解决g-C3N4光催化剂活性低的缺点,本发明提供了一种在可见光条件下增强g-C3N4光催化活性,由N,N-二甲基甲酰胺改性的g-C3N4光催化剂及其制备方法。
为了达到上述目的本发明是通过以下技术方案来实现的:
本发明是一种氮掺杂改性的g-C3N4光催化剂,由N,N-二甲基甲酰胺(DMF)与尿素混合处理得到的CNU-DMF光催化剂。
一种氮掺杂改性的g-C3N4光催化剂制备方法,制备步骤如下:
(1)将尿素与DMF混合均匀,制得前驱体;
(2)将步骤1中得到的前驱体放入坩埚中,并将坩埚置于马弗炉中煅烧,煅烧温度为500~600℃,并保温2~4h;
(3)将步骤2中煅烧后得到的固体空冷至室温,将其放入玛瑙研钵中研磨,研磨时间为10~20min,即得到CNU-DMF光催化剂,并密封储存。
本发明的进一步改进在于:步骤1中所用的尿素和DMF的质量比为1∶(0.5~3)。
本发明的进一步改进在于:步骤2中马弗炉内温度从室温升温至500~600℃,升温速率为2~8℃/min。
本发明的有益效果是:
(1)本发明制备工艺简单、生产成本低、容易操作、原料来源充足,CNU-DMF光催化剂稳定性高,不易造成水体二次污染,在实际应用方面有很大的潜力。
(2)与原始g-C3N4相比,通过DMF改性的g-C3N4具有更大的比表面积,光吸收能力显著增强,并且光生电子-空穴复合率降低,光催化活性得到明显的提高。在可见光条件下能够高效光催化裂解水制氢。
附图说明
图1是实施例1-5中CNU-DMF光催化剂与g-C3N4的XRD图谱;
图2为实施例3中CNU-DMF光催化剂与g-C3N4的XPS图谱;
图3为实施例1-5中CNU-DMF光催化剂与g-C3N4的固体紫外图谱;
图4为实施例3中CNU-DMF光催化剂的与g-C3N4的BET图谱;
图5为实施例3中CNU-DMF光催化剂与g-C3N4的PL图谱;
图6为实施例3中CNU-DMF光催化剂与g-C3N4的光电流和阻抗图谱;
图7为实施例1-5中CNU-DMF光催化剂与g-C3N4的光催化裂解水制氢性能图谱。
具体实施方式
为了加强对本发明的理解,下面将结合附图和实施例对本发明作进一步描述,以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
实施例1
称取10g和5g DMF混合均匀放入坩埚,然后将坩埚置于马弗炉中,从室温加热到550℃,升温速率为5℃/min,在550℃保温3h后空冷至室温,最后再将煅烧后的固体粉末放置于玛瑙研钵中研磨15min,即得到CNU-DMF5,密闭封存。
实施例2
称取10g尿素和7.5g DMF混合均匀放入坩埚,制备步骤同上。
实施例3
称取10g尿素和10g DMF混合均匀放入坩埚,制备步骤同上。
实施例4
称取10g尿素和15g DMF混合均匀放入坩埚,制备步骤同上。
实施例5
称取10g尿素和20g DMF混合均匀放入坩埚,制备步骤同上。
对实施例1-5中CNU-DMF光催化剂与g-C3N4进行XRD表征。使用具有CuKα辐射,其λ为0.1540558nm的推进型XRD衍射仪记录样品的粉末X射线衍射图案,数据收集采用θ/2θ扫描模式,在10°到70°范围内连续扫描完成,扫描速度为7°/min。所有质量比的CNU-DMF光催化剂在27.4°显示出g-C3N4的特征峰(图1a)。值得注意的是,在DMF(图1b)修饰后会出现向较小角度方向的轻微偏斜,说明氮掺杂的引入会导致填料扰动和单层波动。
用X射线光电子能谱(XPS)分析了DMF对g-C3N4化学键合性质的影响。图2a所示的全扫描光谱表明g-C3N4和CNU-DMF10样品中都存在C和N元素,并伴随少量O元素。如图2b所示,g-C3N4的C1sXPS谱以284.7和288.1eV的结合能为中心,可归因于石墨碳原子和sp2杂化碳。CNU-DMF10的C1s峰分别向较低的结合能位置移动0.1和0.2eV。如图2c所示,g-C3N4在404.3eV处的N1s峰可归属于π-激发、-NH2基团或N-N键,其面积小于CNU-DMF10(404.2eV)。在404.2eV处峰面积的增加可归因于N-N键,这意味着C原子被N原子取代。从有机元素分析(图2d)来看,CNU-DMF10的N/C原子比高于g-C3N4,进一步证明CNU-DMF 10确实是通过DMF改性而富氮的。
用紫外漫反射光谱研究了g-C3N4和实施例1-5中的CNU-DMF光催化剂(图3),可以发现与g-C3N4相比,所有质量比的CNU-DMF光催化剂在可见光区域的光吸收均有提高,这表明CNU-DMF光催化剂在可见光照射下有更好的光催化活性。
图4显示的是g-C3N4和实施例4中的CNU-DMF光催化剂的BET图谱。可以发现g-C3N4经过DMF改性之后,比表面积得到了有效的提高,这表明可以更好的利用光能,促进光催化活性。
图5显示的是g-C3N4和实施例4中的CNU-DMF光催化剂的PL图谱。通常,光致发光强度越大,电子空穴对的复合率越高,光催化剂的光催化活性越低。可以发现CNU-DMF光催化剂的荧光强度明显小于未改性的g-C3N4,这表明g-C3N4经过DMF改性之后,光生电子-空穴复合率明显降低,这有利于光催化活性的提高。
图6显示的是g-C3N4和实施例4中的CNU-DMF光催化剂的光电流和阻抗图谱。在图6a中光电流响应证实了DMF对于g-C3N4的改性对降低光生电子-空穴复合率具有重要作用。此外,电化学阻抗图谱可以提供有关光电电极界面电荷转移行为的信息(图6b)。一般情况下,半圆半径越小,电荷转移电阻越小,说明光生电子空穴对的分离和传输速度更快。CNU-DMF光催化剂的半圆半径远小于未改性g-C3N4。通过电化学测试,再次证实了DMF对g-C3N4内光生电子-空穴的分离起到了良好的效果。
图7显示的是g-C3N4和实施例1-5中的CNU-DMF光催化剂的制氢性能图谱。在连续4h的可见光照射下,可以发现与g-C3N4相比,所有质量比的CNU-DMF光催化剂的制氢率都得到了明显的提高,其中,实施例4中的DMF光催化剂的制氢速率最好(275μmol/h)。
Claims (5)
1.一种氮掺杂改性的g-C3N4光催化剂,其特征在于:由N,N-二甲基甲酰胺(DMF)与尿素混合处理得到的CNU-DMF光催化剂。
2.一种氮掺杂改性的g-C3N4光催化剂的制备方法,其特征在于:制备步骤如下:
S1:将尿素与DMF混合均匀,制得前驱体;
S2:将前驱体煅烧;
S3:冷却至室温;
S4:研磨。
3.根据权利要求2所述一种氮掺杂改性的g-C3N4光催化剂的制备方法,其特征在于:S1中所用的尿素和DMF的质量比为1∶(0.5~2)。
4.根据权利要求2所述一种氮掺杂改性的g-C3N4光催化剂的制备方法,其特征在于:S2中煅烧温度为500~600℃,并保温2~4h。
5.根据权利要求2所述一种氮掺杂改性的g-C3N4光催化剂的制备方法,其特征在于:S2中煅烧温度从室温升温至500~600℃,升温速率为2~8℃/min。
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CN111318297A (zh) * | 2020-02-24 | 2020-06-23 | 江苏大学 | 一种高亲水性g-C3N4及制备方法和用途 |
CN114100656A (zh) * | 2021-11-16 | 2022-03-01 | 武汉工程大学 | 一种s-cn-d同质纳米异质结的制备方法 |
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