CN109569669A - 类海绵状单晶多孔Bi5O7I纳米片光催化剂及其制备方法 - Google Patents
类海绵状单晶多孔Bi5O7I纳米片光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种类海绵状单晶多孔Bi5O7I纳米片光催化剂及其制备方法。所述制备方法包括以下步骤:1)将聚乙烯吡咯烷酮和形貌调整剂加入至有机溶剂中,搅拌至溶解完全,并加入碘源和铋源,获得前驱体溶液;2)将步骤1)获得的所述前驱体溶液在100‑180℃下进行水热反应,得到所述BiOI纳米片;3)将所述BiOI纳米片以1‑10℃/min的升温速率升温至200‑700℃,并保温煅烧20‑180min,之后自然冷却至室温得到Bi5O7I。提高了Bi5O7I在光催化反应中的效率。此外,本发明还提出了由上述方法制备得到类海绵状单晶多孔Bi5O7I纳米片光催化剂。
Description
技术领域
本发明涉及材料制备领域,尤其涉及一种类海绵状单晶多孔Bi5O7I纳米片光催化剂及其制备方法。
背景技术
近年来,纳米功能材料在解决能源与环境问题方面展现出巨大的优势。其中,多孔材料由于其具有规则排列和大小可调的孔道结构,在机械、吸附、催化和生物活性等方面展现独特性能,备受国际诸多学科领域学者重视,迅速成为跨学科研究的焦点和热点。铋基氧化物作为重要的功能材料,在电子陶瓷材料、光电转化材料以及药物材料等方面有着重要的作用。其中Bi5O7I作为BiOI一种结构衍生产物在光催化降解有机污染物方面展现出巨大优势。相比BiOI材料,Bi5O7I具有较宽的带隙值(2.83-2.94eV)使其具有较强的光催化氧化性能。其次Bi5O7I具有较好的结晶性能够有效减弱电子跨界面传输阻抗,有利于光生电子的有效传输。
目前,Bi5O7I材料的制备方法主要包括水热法、溶剂热和固相烧结法。通过以上方法制备的样品大多数颗粒粒径较大、比表面积小、反应活性位点数量较少,光催化活性相对较弱。众所周知,形貌对于光催化材料的光吸收、电子与空穴分离以及活性位点暴露调控至关重要。二维光催化材料能够减小体相电子向表面迁移距离,有效促进电子与空穴分离,有利于改善光催化活性。目前所报道的Bi5O7I光催化材料形貌主要有纳米棒,微米球/花状球,片状,块状结构。在这些报道的形貌中,纳米棒、块状形貌不利于体相电子和空穴分离;微米球/花状球形貌虽然能够增强对光的吸收但是不利于电子与空穴分离;常规片状结构虽然促进了电子与空穴体相分离但其比表面较小,表面暴露反应活性位点数量少,也不利于大幅度改善光催化反应速率。
发明内容
本发明所要解决的技术问题是:Bi5O7I光催化剂光催化活性低的技术问题。
为解决上述技术问题,本发明提出了一种类海绵状单晶多孔Bi5O7I纳米片光催化剂及其制备方法。
本发明提出一种Bi5O7I光催化剂的制备方法,包括以下步骤:
1)将聚乙烯吡咯烷酮和形貌调整剂加入至有机溶剂中,搅拌至溶解完全,并加入碘源和铋源,获得前驱体溶液;
2)将步骤1)获得的所述前驱体溶液在100-180℃下进行水热反应,得到均匀分散的所述BiOI纳米片;
3)将步骤2)得到的所述BiOI纳米片以1-10℃/min的升温速率升温至200-700℃,并保温煅烧20-180min,之后自然冷却至室温得到Bi5O7I。
优选地,在步骤1)中,所述形貌调整剂包括聚乙烯亚胺;
优选地,所述有机溶剂包括乙二醇溶剂。
优选地,在步骤1)中,所述碘源包括碘化钾、碘化钠和碘化锂的一种或多种。
优选地,所述铋源包括硝酸铋、氯化铋、硫酸铋和枸橼酸铋钾的一种或多种。
优选地,在步骤1)中,所述聚乙烯吡咯烷酮和所述聚乙烯亚胺加入至所述有机溶剂中,搅拌至溶解完全后,所述聚乙烯吡咯烷酮和所述聚乙烯亚胺的浓度分别为0.1~15g/L。
优选地,在步骤1)中所述碘源中的碘元素与所述铋源中的铋元素的摩尔比为(0.001~0.5):(0.001~0.5)。
优选地,在步骤2)中,所述水热反应的时间为1~20h。
优选地,在步骤2)中,水热反应之后还包括离心干燥处理得到所述BiOI纳米片。
本发明还包括一种上述所述的制备方法制备的类海绵状单晶多孔Bi5O7I纳米片光催化剂。
本发明与现有技术对比的有益效果包括:将聚乙烯吡咯烷酮和形貌调整剂加入至有机溶剂中,搅拌至溶解完全,并加入碘源和铋源,获得前驱体溶液,之后在100-180℃下进行水热反应,得到均匀分散的所述BiOI纳米片,制备的BiOI纳米片表面残留有有机质,将所述BiOI纳米片以1-10℃/min的升温速率升温至200-700℃,并保温煅烧20-180min,之后自然冷却至室温,残留的有机质在煅烧过程中有助于多孔结构的产生,加上煅烧过程中碘的挥发,进一步有利于多孔结构的产生,从而得到类海绵二维片状单晶多孔结构的Bi5O7I,Bi5O7I的二维结构可以提高光生电子和空穴的分离效率;单晶晶型使光生电子传输阻抗小;类海绵状多孔结构中独特的孔道结构不但能够促进反应活性位点的暴露,同时光线在孔道内的多重散射折射延长了光程差,提高了对光的利用率;多孔结构对反应底物具有较强的吸附能力,提高反应底物与催化剂接触几率,加速反应传质过程,从而提高了Bi5O7I在光催化反应中的效率。
附图说明
通过参考附图会更加清楚的理解本发明的特征和优点,附图是示意性的而不应理解为对本发明进行任何限制,在附图中:
图1为本发明实施例1合成的类海绵状单晶多孔Bi5O7I纳米片光催化剂的XRD图。
图2为本发明实施例1合成的类海绵状单晶多孔Bi5O7I纳米片光催化剂的SEM图。
图3为本发明实施例1合成的类海绵状单晶多孔Bi5O7I纳米片光催化剂的TEM图。
图4为本发明实施例1合成的类海绵状单晶多孔Bi5O7I纳米片光催化剂的电子衍射图。
图5为本发明实施例1合成的类海绵状单晶多孔Bi5O7I纳米片光催化剂的HRTEM图。
图6为本发明应用例1中类海绵状单晶多孔Bi5O7I纳米片光催化降解罗丹明B效果图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本发明内涵的情况下做类似改进,因此本发明不受下面公开的具体实施的限制。
实施例1
本实施例的类海绵状单晶多孔Bi5O7I纳米片光催化剂通过以下步骤制备得到:
将0.0715g聚乙烯吡咯烷酮、0.1785g聚乙烯亚胺加入到50mL乙二醇溶液中,搅拌至溶解完全;并加入0.664g碘化钾和1.94g硝酸铋,搅拌5-30min获得褐色透明溶液。将所述褐色透明溶液转移至水热反应釜中,在100℃条件下水热反应20h,之后自然冷却至室温,经过离心、干燥获得分散均匀的BiOI纳米片。
将所获得BiOI纳米片转移至马弗炉中以5℃/min的升温速率升温至500℃,保温煅烧60min,自然冷却至室温获得类海绵状单晶多孔Bi5O7I纳米片。
从图1可以得知,所制备类海绵状单晶多孔纳米片的衍射峰与标准Bi5O7I晶体衍射卡片(JCPDS:40-0548)完全吻合且衍射峰强度较高,不存在其他杂相衍射峰。这证明所制备的类海绵状单晶多孔纳米片为Bi5O7I晶体,结晶度高,不存在其他杂质晶相。
从图2可以得知,制备的Bi5O7I为片状结构,片层厚度为50-80nm,片层表面和体相存在大量均匀分布孔洞,孔径尺寸分布均匀,整体呈现类似海绵结构。
图3的TEM图表明纳米片Bi5O7I为多孔结构,孔径尺寸较均匀;多孔重叠现象证明片层体相存在大量孔洞,进一步证实类海绵状结构存在。
图4电子衍射图谱中类矩形规则排列衍射斑点证明所制备类海绵状多孔纳米片为单晶结构,此种结构有利于光生电子在纳米片中传输。
图5的HRTEM图中排列规整的晶格条纹进一步说明所制备材料为单晶结构,并且从图中可以看出孔结构轮廓,这与SEM图中多孔结构相对应。
实施例2
本实施例的类海绵状单晶多孔Bi5O7I纳米片光催化剂通过以下步骤制备得到:
将1.0g聚乙烯吡咯烷酮、0.5g聚乙烯亚胺加入到70mL乙二醇溶液中,搅拌至溶解完全;并加入0.75g碘化钠和0.63g氯化铋,搅拌5-30min获得褐色透明溶液。将所述褐色透明溶液溶液转移至水热反应釜中,在160℃条件下水热反应12h,之后自然冷却至室温,经过离心、干燥获得分散均匀的BiOI纳米片。
将所获得BiOI纳米片转移至马弗炉中以1℃/min的升温速率升温至450℃,保温煅烧30min,自然冷却至室温获得类海绵状单晶多孔Bi5O7I纳米片。
实施例3
本实施例的类海绵状单晶多孔Bi5O7I纳米片光催化剂通过以下步骤制备得到:
将0.043g聚乙烯吡咯烷酮、0.05g聚乙烯亚胺加入到30mL乙二醇溶液中,搅拌至溶解完全;并加入0.013g碘化锂和0.018g硫酸铋,搅拌5-30min获得褐色透明溶液。将所述褐色透明溶液溶液转移至水热反应釜中,在160℃条件下水热反应6h,之后自然冷却至室温,经过离心、干燥获得分散均匀的BiOI纳米片。所获得BiOI纳米片转移至马弗炉中以6℃/min的升温速率升温至400℃,保温煅烧180min,自然冷却至室温获得类海绵状单晶多孔Bi5O7I纳米片。
实施例4
本实施例的类海绵状单晶多孔Bi5O7I纳米片光催化剂通过以下步骤制备得到:
将0.357g聚乙烯吡咯烷酮、0.0715g聚乙烯亚胺加入到50mL乙二醇溶液中,搅拌至溶解完全;加入0.33g碘化钾和0.7g枸橼酸铋钾,搅拌5-30min获得褐色透明溶液。将所述褐色透明溶液转移至水热反应釜中,在180℃条件下水热反应3h,之后自然冷却至室温,经过离心、干燥获得分散均匀的BiOI纳米片。所获得的BiOI纳米片转移至马弗炉中以10℃/min的升温速率升温至500℃,保温煅烧60min,自然冷却至室温获得类海绵状单晶多孔Bi5O7I纳米片。
应用例1
罗丹明B的光催化降解
将实施例1制备的类海绵状单晶多孔Bi5O7I纳米片催化剂应用于罗丹明B的光催化氧化降解实验,所用的模拟光源为300W的氙灯(加入420nm滤光片),罗丹明B溶液的浓度为20mg/L,步骤如下:首先把10mg实施例1制备的类海绵状多孔Bi5O7I纳米片催化剂加入到40mL的罗丹明B溶液中,然后避光磁力搅拌60min;打开光源,每隔10min取5ml溶液,离心分离取上层清液,用分光光度计测试其吸光度。结合图6,从可见光降解罗丹明B染料实验结果可以看出,经过50min几乎所有罗丹明B被完全降解,降解效率为99.24%,类海绵状单晶多孔Bi5O7I纳米片具有优异的光催化性能。
本发明的有益效果还包括:
1)合成过程简单、前驱体廉价易得、不需添加模板剂,也无需复杂设备,易操作、重复性操作强。
2)产品微观形貌均一、单晶晶型、孔尺寸分布范围窄,产率高,在光催化、吸附、气敏、电池等领域具有较高的应用价值。
3)本发明提出的方法与传统的制备Bi5O7I光催化剂合成法相比,步骤更加简单,操作更加方便,工艺更容易掌握。
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。
Claims (10)
1.一种类海绵状单晶多孔Bi5O7I纳米片光催化剂的制备方法,其特征在于,包括以下步骤:
1)将聚乙烯吡咯烷酮和形貌调整剂加入至有机溶剂中,搅拌至溶解完全,并加入碘源和铋源,获得前驱体溶液;
2)将步骤1)获得的所述前驱体溶液在100-180℃下进行水热反应,得到均匀分散的所述BiOI纳米片;
3)将步骤2)得到的所述BiOI纳米片以1-10℃/min的升温速率升温至200-700℃,并保温煅烧20-180min,之后自然冷却至室温得到所述类海绵状单晶多孔Bi5O7I纳米片。
2.根据权利要求1所述的制备方法,其特征在于,在步骤1)中,所述形貌调整剂包括聚乙烯亚胺。
3.根据权利要求1所述的制备方法,其特征在于,在步骤1)中,所述有机溶剂包括乙二醇溶剂。
4.根据权利要求1所述的制备方法,其特征在于,在步骤1)中,所述碘源包括碘化钾、碘化钠和碘化锂的一种或多种。
5.根据权利要求1所述的制备方法,其特征在于,在步骤1)中,所述铋源包括硝酸铋、氯化铋、硫酸铋和枸橼酸铋钾的一种或多种。
6.根据权利要求2所述的制备方法,其特征在于,在步骤1)中,所述聚乙烯吡咯烷酮和所述聚乙烯亚胺加入至所述有机溶剂中,搅拌至溶解完全后,所述聚乙烯吡咯烷酮和所述聚乙烯亚胺的浓度分别为0.1~15g/L。
7.根据权利要求1所述的制备方法,其特征在于,在步骤1)中所述碘源中的碘元素与所述铋源中的铋元素的摩尔比为(0.001~0.5):(0.001~0.5)。
8.根据权利要求2所述的制备方法,其特征在于,在步骤2)中,所述水热反应的时间为1~20h。
9.根据权利要求2所述的制备方法,其特征在于,在步骤2)中,水热反应之后还包括离心干燥处理得到所述BiOI纳米片。
10.一种如权利要求1-9任一项所述的制备方法制备的类海绵状单晶多孔Bi5O7I纳米片光催化剂。
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