CN113998689B - 一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法及其应用 - Google Patents
一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法及其应用 Download PDFInfo
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Abstract
本发明属于碳材料制备技术领域,一种基于非共价键作用构筑g‑C3N4量子点/碳复合材料的方法及其应用,其中构筑方法,包括以下步骤:利用高温热聚合法,以富氮材料为前驱体制备g‑C3N4;对上述g‑C3N4利用低温预处理结合液相剥离工艺制备g‑C3N4量子点;采用机械搅拌结合高速离心工艺,使具有含氮活性基团的g‑C3N4量子点与导电性良好的碳材料通过非共价键π‑π堆积相互作用得到g‑C3N4量子点/碳复合材料。该方法具有制备工艺简单、条件温和、低能耗、高效、低成本等特点。本发明构筑的g‑C3N4量子点/碳复合材料相比于市购Pt电极表现出了更高的I3 ‑催化活性能,是一种在染料敏化太阳能电池中具有广泛应用前景的材料。
Description
技术领域
本发明涉及一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法及其应用,属于碳材料制备技术领域。
背景技术
染料敏化太阳能电池(DSSCs)作为一种新型的太阳能电池受到研究者们的广泛关注。DSSCs主要由光阳极、对电极和含氧化还原电对的电解液三部分组成,其中,对电极作为DSSCs重要组成之一,主要起到收集外电路电子和催化I3 -还原的作用。传统的对电极材料主要是贵金属Pt,但Pt具有储量有限、成本高等缺点,极大地限制了DSSCs大规模应用。因此,开发低成本且催化性能优异的对电极材料一直是研究的热点。已有研究显示,碳材料因其来源广泛、价格低廉、导电性好、稳定性高及良好的催化活性等特点,在取代Pt对电极方面显示出极大的潜力。迄今为止,石墨烯、碳纳米管、碳纳米带等被广泛用作DSSCs的对电极材料。随着研究的深入,科学家们发现具有化学惰性的基面,是致使碳材料整体性能低的主要原因,而理想的对电极材料应兼具高的催化活性和导电性。为了进一步增强碳材料的催化性能,利用杂原子掺杂(N、S、P等)来诱导非本征缺陷,从而构筑新的活性位点以增强其催化活性是常用的有效途径。
大量理论计算和实验研究表明,在众多杂原子中,氮原子与碳原子的原子半径接近,从热力学上来讲,更有利于取代碳原子进行掺杂。另外,氮原子的电负性(3.04)大于碳原子(2.55),氮原子额外的孤对电子就可以为sp2杂化的碳骨架离域π体系提供电子,以改善其电子结构进而增强其化学反应活性。在氮掺杂碳材料中,不同形式的含氮官能团对碳材料的电荷分布以及电子结构产生不同影响。理论和实验研究表明,吡啶氮是提高其I3 -还原性能的主要因素之一。但是在碳氮共价键成键时,长程有序碳骨架中的碳碳键和氮源中的氮氢键或碳氮键发生断裂,这就需要额外能量的输入。因此,不论是利用原位掺杂策略的模板法、直接热解法、化学反应法还是利用间接掺杂策略的干法、湿法在制备含氮碳材料的过程中,都需要高温处理步骤,打断部分原有的键,最终导致能耗较高。而与共价键作用(Ebond=150~1000kJ/mol)相比,非共价键π-π堆积作用所需能量更小(Ebond<50kJ/mol),而且非共价键π-π堆积作用不仅不会对碳材料的结构造成破坏,还会保留碳材料的本征结构性质。综上所述,利用非共价键作用开发制备工艺简单、条件温和且高效的含氮碳复合材料成为染料敏化太阳能电池对电极材料亟需解决的问题。
与氮掺杂碳材料具有类似结构的石墨相氮化碳(g-C3N4)是一种新型的无机非金属催化剂,具有类似石墨烯的二维结构,C、N原子均发生sp2杂化,且所有原子的p轨道互相重叠形成离域π键。依据其原子结构可知,C/N原子比例为0.75,即氮含量约为57.14%,且大部分为吡啶氮,丰富的含氮活性基团能够为电化学反应提供较多的活性位点,是很有前景的电催化剂。但是由于g-C3N4导电性差、比表面积小、电子迁移率低,使其催化活性仍不理想。
针对碳材料活性位点较少和石墨相氮化碳导电性差、比表面积小的问题,本发明以碳材料为导电基底利用非共价键作用与石墨相氮化碳相结合,充分发挥两种材料的协同作用。开发制备工艺简单、能耗低、绿色环保的g-C3N4量子点/碳复合材料对制备低成本、高性能的碳基材料具有重要的指导意义,为推进DSSCs商业化进程提供了理论指导。
发明内容
为了克服现有技术中存在的不足,本发明目的是提供一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法及其应用。该方法,利用非共价键表面修饰策略,使带有含氮活性基团的g-C3N4量子点与导电性良好的碳材料通过非共价键π-π相互作用堆积在一起,制备g-C3N4量子点/碳复合材料,该复合材料集成g-C3N4量子点优异的催化性能和碳材料良好的导电性能,能够有效催化I3 -还原,在染料敏化太阳能电池对电极I3 -还原方面表现出优异的性能。
为了实现上述发明目的,解决已有技术中所存在的问题,本发明采取的技术方案是:一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法,包括以下步骤:
步骤1、利用高温热聚合法,将6~10g富氮材料作为前驱体在450~600℃的空气或氮气气氛下高温煅烧2~4h,取出研磨得到g-C3N4粉体,所述富氮材料选自三聚氰胺、尿素或双氰胺中的一种;
步骤2、将步骤1得到的g-C3N4粉体置于离心管中,并向其中缓慢加入液氮,再将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理10~90min;
步骤3、将步骤2处理后的g-C3N4粉体加入到分散剂中液相剥离1~5h,所述g-C3N4粉体质量与分散剂体积之比为1~4mg/mL,所述液相剥离所用分散剂选自乙醇、异丙醇、丙酮、二甲基甲酰胺或水中的一种或二种;
步骤4、将步骤3剥离后的混合物在转速为6000~12000rpm的离心机中离心5~15min,收集离心后的上层液体,采用截留分子量为200的透析袋透析3~5天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点;
步骤5、将步骤4得到的g-C3N4量子点与碳材料加入蒸馏水中磁力搅拌2~5h,两种材料通过非共价键π-π堆积作用耦合,所述g-C3N4量子点、碳材料及蒸馏水的质量比为1:10~50:10~50,所述碳材料选自羧基化多壁碳纳米管、羧基化单壁碳纳米管、碳纳米带或石墨烯中的一种;
步骤6、将步骤5得到的固液混合物在转速为8000~20000rpm的离心机中离心5~15min,收集下层物质,经冻干后得到g-C3N4量子点/碳复合材料,
所述g-C3N4量子点/碳复合材料中g-C3N4量子点通过非共价键π-π堆积作用修饰在碳材料的表面,g-C3N4量子点/碳复合材料含有的元素为:碳、氮和氧元素,其中氮元素的原子百分比为2~13%。
所述方法构筑g-C3N4量子点/碳复合材料在染料敏化太阳能电池中的应用。
本发明有益效果是:一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法及其应用,其中构筑方法包括以下步骤:(1)利用高温热聚合法,将富氮材料作为前驱体在空气或氮气气氛下高温煅烧,取出研磨得到g-C3N4粉体,(2)将步骤1得到的g-C3N4粉体置于离心管中,并向其中缓慢加入液氮,再将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,进行低温预处理,(3)将步骤2处理后的g-C3N4粉体加入到分散剂中进行液相剥离,(4)将步骤3剥离后的混合物在离心机中离心,收集离心后的上层液体,透析以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点;(5)将步骤4得到的g-C3N4量子点与碳材料加入蒸馏水中磁力搅拌,(6)将步骤5得到的固液混合物在离心机中离心,收集下层物质,经冻干后得到g-C3N4量子点/碳复合材料。本发明具有以下优点:一是,本发明利用碳材料与g-C3N4量子点之间的非共价键π-π堆积作用,采用简单的机械搅拌结合高速离心工艺制备含氮的g-C3N4量子点/碳复合材料。该方法工艺简单、条件温和、成本低,与形成碳氮共价键的含氮碳材料制备方法相比,非共价键所需能量低,且不会破坏碳材料结构和本征性质。二是,本发明通过调节离心机转速实现g-C3N4量子点/碳复合材料中氮含量的调控。三是,本发明制备g-C3N4量子点的方法即低温预处理结合液相剥离,与常用的液相剥离相比较,低温预处理时温度骤冷,受应力作用在二维粉末中形成小裂纹,这些裂缝,作为毛细血管,在液相剥离时允许分散剂渗透。低温预处理使得液相剥离更容易得到量子点,从而对分散剂依赖性减弱,可选择低沸点分散剂。低温预处理后,温度恢复过程中的热膨胀有助于减弱二维材料的层内范德华力。四是,本发明中,除液相剥离的分散剂外,没有其它有机试剂,制备过程不会产生废气,环境友好。
附图说明
图1是实施例1中制备的g-C3N4量子点横向尺寸分布图。
图中:(a)表示g-C3N4量子点的TEM电镜图,(b)表示g-C3N4量子点横向尺寸统计柱状图。
图2是实施例2中制备的g-C3N4量子点/羧基化多壁碳纳米管复合材料的形貌结构图。
图中:(a)表示g-C3N4量子点/羧基化多壁碳纳米管复合材料的TEM电镜图,(b)表示g-C3N4量子点/羧基化多壁碳纳米管复合材料的HRTEM电镜图,(c)表示其局部放大的HRTEM电镜图。
图3是实施例3中制备的g-C3N4量子点/羧基化单壁碳纳米管复合材料(CNQDs/SWCNT)及市购Pt电极的J-V曲线图。
图4是实施例4制备的g-C3N4量子点/石墨烯复合材料(CNQDs/G)和实施例5制备的g-C3N4量子点/碳纳米带复合材料(CNQDs/CNB)的XPS谱图。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1
步骤1、称取10g三聚氰胺在550℃的空气气氛下高温煅烧4h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1200mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理60min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到含200mL水和200mL异丙醇的溶液中,液相剥离4h。步骤4、将步骤3剥离后的混合物在转速为12000rpm的离心机中离心10min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、称取步骤4中的g-C3N4量子点2mg及羧基化多壁碳纳米管100mg,加入到100mg蒸馏水中,混合后磁力搅拌4h。步骤6、将步骤5中得到的固液混合物在转速为17000rpm的离心机中离心10min,收集下层物质,经冻干后得到g-C3N4量子点/羧基化多壁碳纳米管复合材料。制备的g-C3N4量子点横向尺寸分布图,如图1所示,图1(a)为g-C3N4量子点的TEM电镜图,图1(b)为g-C3N4量子点横向尺寸统计柱状图,从图中统计结果可看出g-C3N4量子点的横向尺寸主要集中在2~5nm之间,平均横向尺寸为3.4nm。
实施例2
步骤1、称取10g三聚氰胺在550℃的空气气氛下高温煅烧4h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1200mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理60min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到含200mL水和200mL异丙醇的溶液中,液相剥离4h。步骤4、将步骤3剥离后的混合物在转速为12000rpm的离心机中离心10min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、称取步骤4中的g-C3N4量子点2mg及羧基化多壁碳纳米管100mg,加入到100mg蒸馏水中,混合后磁力搅拌4h。步骤6、将步骤5中得到的固液混合物在转速为20000rpm的离心机中离心10min,收集下层物质,经冻干后得到g-C3N4量子点/羧基化多壁碳纳米管复合材料。其形貌结构图,如图2所示,从图2(a)-2(b)可以看出g-C3N4量子点耦合在羧基化多壁碳纳米管的表面,从图2(c)可以看出晶面间距0.21nm对应g-C3N4量子点的100晶面,晶面间距0.34nm对应碳管的晶面间距,证明g-C3N4量子点成功通过非共价键π-π堆积作用修饰在羧基化多壁碳纳米管的表面。
实施例3
步骤1、称取6g尿素在500℃的氮气气氛下高温煅烧3h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1600mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理30min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到800mL丙酮的溶液中,液相剥离3h。步骤4、将步骤3剥离后的混合物在转速为11000rpm的离心机中离心15min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、称取步骤4中的g-C3N4量子点3mg及羧基化单壁碳纳米管80mg加入到100mg蒸馏水中,混合后磁力搅拌2h。步骤6、将步骤5中得到的固液混合物在转速为17000rpm的离心机中离心15min,收集下层物质,经冻干后得到g-C3N4量子点/羧基化单壁碳纳米管复合材料。
以实施例3制备的g-C3N4量子点/羧基化单壁碳纳米管复合材料为对电极组装染料敏化太阳能电池,测试其光电转化效率(PCE),具体的测试方法为:(1)将30mg g-C3N4量子点/羧基化单壁碳纳米管复合材料与0.5mL粘结剂(m乙基纤维素:m松油醇:m乙醇=1:8:9)用研钵研磨30min得到均匀浆料,采用刮涂法将浆料涂抹到FTO导电玻璃上;最后将涂有浆料的FTO玻璃转移至管式炉中于氮气气氛下,按2℃min-1的升温速率将炉温升至500℃,维持30min,得到对电极。Pt对电极为商业化购买得到。(2)所用到的TiO2光阳极为商业购买得到,将购买的TiO2光阳极放置于马弗炉中于500℃下煅烧30min,等炉温降至100℃时,将电极浸泡在5×10-4mol/L的N719乙醇溶液液中,浸泡时间为20h;将吸附有染料的TiO2电极用吹风机快速吹干、备用。(3)将光阳极和对电极用厚度为45μm的沙林膜回字框隔开,然后置于热压机下,在0.4Mpa、125℃下维持20s。待温度降至室温,将商业购买的电解质通过对电极的小孔真空注入到电池内部。最后用沙林膜将小孔封堵,即得到具有三明治结构的染料敏化太阳能电池。电池的活性面积为0.16cm2。(4)采用美国Newport公司生产的94032A型AAA级太阳光模拟器对(3)中组装好的电池进行J-V测试。测试条件为AM 1.5模拟太阳光,光照强度为100mW cm-2。测试电压范围:0-0.8V。
图3为以g-C3N4量子点/羧基化单壁碳纳米管复合材料(CNQDs/SWCNT)为对电极及市购Pt对电极的J-V曲线图,如图3所示,它所对应的详细光电参数如表1所示,由表1可以看出在以上两种材料作为对电极所组装的染料敏化太阳能电池中,g-C3N4量子点/羧基化单壁碳纳米管复合材料(CNQDs/SWCNT)作为对电极兼具良好的导电性和电催化性能,其光电转化效率(8.35%)优于市购Pt对电极(7.87%)。
表1
CE | J<sub>sc</sub>(mA cm<sup>-2</sup>) | V<sub>oc</sub>(V) | FF(%) | PCE(%) |
CNQDs/SWCNT | 15.29±0.11 | 0.73±0.01 | 74.83±0.52 | 8.35±0.06 |
Pt | 14.15±0.06 | 0.75±0.01 | 74.20±0.91 | 7.87±0.04 |
注:每个参数为组装10块电池测得的平均值。
实施例4
步骤1、称取8g三聚氰胺在550℃的氮气气氛下高温煅烧4h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1200mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理90min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到400mL乙醇的溶液中,液相剥离5h。步骤4、将步骤3剥离后的混合物在转速为10000rpm的离心机中离心15min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、分别称取两份步骤4中的g-C3N4量子点3mg及石墨烯50mg加入到80mg蒸馏水中,混合后磁力搅拌5h。步骤6、将步骤5中得到的固液混合物分别在转速为9000rpm和17000rpm的离心机中离心10min,收集下层物质,经冻干后分别得到g-C3N4量子点/石墨烯复合材料(CNQDs/G-9000、CNQDs/G-17000)。两种不同转速的g-C3N4量子点/石墨烯复合材料(CNQDs/G-9000、CNQDs/G-17000)及所用石墨烯(G)的XPS谱图,如图4所示,从图中可以看出,原始的石墨烯中不含氮,而复合材料中随着离心机转速的增加(9000rpm、17000rpm),氮原子的含量增加(2.1%、5.7%)。证明了两种物质成功耦合,并且可以通过调节离心机的转速调控复合材料中氮原子的含量。
实施例5
步骤1、称取7g双氰胺在550℃的空气气氛下高温煅烧3h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1600mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理40min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到400mL二甲基甲酰胺的溶液中,液相剥离3h。步骤4、将步骤3剥离后的混合物在转速为12000rpm的离心机中离心15min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、称取步骤4中的g-C3N4量子点4mg及碳纳米带90mg加入到80mg蒸馏水中,混合后磁力搅拌3h。步骤6、将步骤5中得到的固液混合物在转速为15000rpm的离心机中离心9min,收集下层物质,经冻干后得到g-C3N4量子点/碳纳米带复合材料(CNQDs/CNB),其XPS谱图,如图4所示,从图中可以看出,复合材料中氮原子的含量为5.2%。
实施例6
步骤1、称取10g三聚氰胺在550℃的空气气氛下高温煅烧4h,取出研磨得到g-C3N4粉体。步骤2、称取步骤1中的g-C3N4粉体1200mg置于离心管中,向其中缓慢加入液氮,将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理60min。步骤3、取出步骤2中预处理后的g-C3N4粉体,加入到含150mL水和150mL异丙醇的溶液中,液相剥离4h。步骤4、将步骤3剥离后的混合物在转速为12000rpm的离心机中离心10min,收集离心后的上层液,采用截留分子量为200的透析袋透析3天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点。步骤5、称取步骤4中的g-C3N4量子点2mg及羧基化单壁碳纳米管100mg加入到100mg蒸馏水中,混合后磁力搅拌3h。步骤6、将步骤5中得到的固液混合物在转速为20000rpm的离心机中离心10min,收集下层物质,经冻干后得到g-C3N4量子点/羧基化单壁碳纳米管复合材料。
Claims (2)
1.一种基于非共价键作用构筑g-C3N4量子点/碳复合材料的方法,其特征在于,包括以下步骤:
步骤1、利用高温热聚合法,将6~10g富氮材料作为前驱体在450~600℃的空气或氮气气氛下高温煅烧2~4h,取出研磨得到g-C3N4粉体,所述富氮材料选自三聚氰胺、尿素或双氰胺中的一种;
步骤2、将步骤1得到的g-C3N4粉体置于离心管中,并向其中缓慢加入液氮,再将离心管放入到盛有液氮的杜瓦瓶中,加上泡沫盖,低温预处理10~90min;
步骤3、将步骤2处理后的g-C3N4粉体加入到分散剂中液相剥离1~5h,所述g-C3N4粉体质量与分散剂体积之比为1~4mg/mL,所述液相剥离所用分散剂选自乙醇、异丙醇、丙酮、二甲基甲酰胺或水中的一种或二种;
步骤4、将步骤3剥离后的混合物在转速为6000~12000rpm的离心机中离心5~15min,收集离心后的上层液体,采用截留分子量为200的透析袋透析3~5天以去除溶剂,透析好的液体经冻干后得到g-C3N4量子点;
步骤5、将步骤4得到的g-C3N4量子点与碳材料加入蒸馏水中磁力搅拌2~5h,两种材料通过非共价键π-π堆积作用耦合,所述g-C3N4量子点、碳材料及蒸馏水的质量比为1:10~50:10~50,所述碳材料选自羧基化多壁碳纳米管、羧基化单壁碳纳米管、碳纳米带或石墨烯中的一种;
步骤6、将步骤5得到的固液混合物在转速为8000~20000rpm的离心机中离心5~15min,收集下层物质,经冻干后得到g-C3N4量子点/碳复合材料,所述g-C3N4量子点/碳复合材料中g-C3N4量子点通过非共价键π-π堆积作用修饰在碳材料的表面,g-C3N4量子点/碳复合材料含有的元素为:碳、氮和氧元素,其中氮元素的原子百分比为2~13%。
2.根据权利要求1所述方法构筑g-C3N4量子点/碳复合材料在染料敏化太阳能电池中的应用。
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