CN111054321A - 一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法 - Google Patents
一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法 Download PDFInfo
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Abstract
本发明涉及一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热‑溶剂热法,属于半导体光催化材料制备技术领域,其特征在于包括以下步骤:以五水合硝酸铋、偏钒酸铵和四水合钼酸铵为金属源,乙二醇和去离子水为混合溶剂,用NaOH调节混合溶液pH值为5;在180℃下反应24h;然后经抽滤、洗涤和烘干,最后于400℃下保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。本发明通过简单调控V/Mo摩尔比,有效实现纺锤形BiVO4/Bi2MoO6复合粉体的制备,具有工艺简单、形貌结构可控、可重复性高等特点。
Description
技术领域
本发明属于半导体光催化材料制备技术领域,具体涉及一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法。
背景技术
随着工业化进程的加快,随之而来的环境问题严重威胁着人类的生存环境。目前处理水污染的方法虽然有一定成效,但也存在着诸多问题,例如:效率低、易产生二次污染、消耗能量高、处理成本高等。相比之下,光催化技术具有效率高、能耗低、无二次污染等优点,从而引起了人们的广泛关注,但目前研究较多的TiO2因其禁带宽度较宽、只能吸收紫外光等缺点限制了其对太阳能的利用率。
而铋系光催化剂的带隙较窄,在可见光范围内有明显的吸收,具有较好的催化活性,因此逐渐成为当今研究的重点。单斜相BiVO4的稳定性好、禁带宽度相对较窄,在可见光照射下具有良好的光催化性能,然而,纯相BiVO4的光生电子空穴对复合率高等问题限制了其实际应用。相关研究表明,通过将两种具有不同能带结构的半导体光催化剂复合来构建异质结构能有效抑制光生电子空穴对的复合几率。刘珊珊等通过固混法制备了质量比为30%BiVO4/g-C3N4复合光催化材料,可见光照射3h后的罗丹明b降解率可达87%(刘珊珊等,化工新型材料, 2017, 45(10): 90-93)。Li等通过光辅助沉积-水热法成功制备了具有高可见光催化性能的新型Ag/BiVO4/rGO杂化复合材料,与纯BiVO4相比,优化后的复合材料表现出更强的光催化性能(M Li, et al. Sci. Total Environ., 2019, 664: 230-239)。
大量研究表明,Bi2MoO6具有独特的层状结构、较窄的禁带宽度,因此有着优良的可见光催化性能,且Bi2MoO6的能带位置与BiVO4的能带位置能较好地匹配,有利于促进光生电子-空穴对的分离。Xu(CQ Xu, et al. Int. J. Mod. Phys. B, 2017, 31: 1744059)和林雪(林雪等, 物理化学学报, 2014, 30(11): 2113-2120)等采用水热法成功合成片状BiVO4/Bi2MoO6复合半导体催化剂,相比于纯相BiVO4和Bi2MoO6样品,复合后样品的光催化性能得到显著提高。
迄今为止,尚无专利和文献报道过制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法。
发明内容
本发明的目的在于提供一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法,本发明制备的纺锤形BiVO4/Bi2MoO6复合粉体由纳米颗粒组装而成,长度为1-2.5μm,宽度为0.3-0.8μm,吸收边界为529nm。
本发明采用的技术方案如下:
步骤1. 在搅拌条件下,将V/Mo摩尔比为2-4:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。
本发明以硝酸铋、偏钒酸铵和钼酸铵为金属源,乙二醇和去离子水为混合溶剂,NaOH为pH调节剂,采用水热-溶剂热法制备纺锤形BiVO4/Bi2MoO6复合粉体。V/Mo摩尔比和乙二醇对纺锤形BiVO4/Bi2MoO6复合粉体的形成起到重要作用。
本发明的有益效果在于:
(1)本发明以乙二醇为结构导向剂,通过调控V/Mo摩尔比,成功制备出纺锤形BiVO4/Bi2MoO6复合粉体;
(2)本发明制备的纺锤形BiVO4/Bi2MoO6复合粉体具有原料廉价易得、工艺简单、形貌和结构可控、可重复性高等优点;
(3)本发明制备的纺锤形BiVO4/Bi2MoO6复合粉体,可以降低光生载流子的复合几率,有效降解水中污染物,在污水处理方面具有优良的应用前景。
附图说明
为了进一步了解本发明,下面以实施例作详细说明,并给出附图描述本发明得到的纺锤形BiVO4/Bi2MoO6复合粉体,其中:
图1为制得的纺锤形BiVO4/Bi2MoO6复合粉体的X射线衍射(XRD)谱图,其中曲线(A)和曲线(B)分别为实施例1和实施例3样品的XRD谱图。
图2为制得的纺锤形BiVO4/Bi2MoO6复合粉体的拉曼光谱(Raman),其中曲线(A)和曲线(B)分别为实施例1和实施例3样品的Raman曲线。
图3为制得的纺锤形BiVO4/Bi2MoO6复合粉体的扫描电子显微镜(SEM)照片,其中图3(A)和3(B)分别为实施例1和实施例3样品的SEM照片。
图4为制得的纺锤形BiVO4/Bi2MoO6复合粉体的紫外-可见漫反射(UV-vis DRS)谱图,其中曲线(A)和曲线(B)分别为实施例1和实施例3样品的UV-vis DRS谱图。
图5为本发明对比例1制得的BiVO4/Bi2MoO6复合粉体的扫描电子显微镜(SEM)照片。
具体实施方式
实施例1:
步骤1. 在搅拌条件下,将V/Mo摩尔比为2:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。
经实施例1制得的纺锤形BiVO4/Bi2MoO6复合粉体的X射线衍射(XRD)谱图如图1中曲线(A)所示,证明了所制备的复合粉体中存在BiVO4物相。为了进一步证明Bi2MoO6物相的存在,对实施例1制备的复合样品进行拉曼光谱(Raman)表征,结果如图2中曲线(A)所示,结果表明,所制备的复合样品中不仅存在BiVO4物相,875cm-1处峰的出现进一步证明了Bi2MoO6物相的存在,表明成功制备得到BiVO4/Bi2MoO6复合粉体。经实施例1制得的纺锤形BiVO4/Bi2MoO6复合粉体的扫描电子显微镜(SEM)照片如图3(A)所示,表明最终制备的BiVO4/Bi2MoO6复合粉体具有典型的纺锤形结构,长度约为1μm,宽度约为0.3μm。经实施例1制得的纺锤形BiVO4/Bi2MoO6复合粉体的紫外-可见漫反射(UV-vis DRS)谱图如图4中曲线(A)所示,表明所制备的复合样品的吸收边界为529nm。
实施例2:
步骤1. 在搅拌条件下,将V/Mo摩尔比为3:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。
实施例3:
步骤1. 在搅拌条件下,将V/Mo摩尔比为4:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。
经实施例3制得的纺锤形BiVO4/Bi2MoO6复合粉体的X射线衍射(XRD)谱图如图1中曲线(B)所示,证明了所制备的复合粉体中存在BiVO4物相。为了进一步证明Bi2MoO6物相的存在,对实施例1制备的复合样品进行拉曼光谱(Raman)表征,结果如图2中曲线(B)所示,结果表明,所制备的复合样品中不仅存在BiVO4物相,875cm-1处峰的出现进一步证明了Bi2MoO6物相的存在,表明成功制备得到BiVO4/Bi2MoO6复合粉体。经实施例3制得的纺锤形BiVO4/Bi2MoO6复合粉体的扫描电子显微镜(SEM)照片如图3(B)所示,表明最终制备的BiVO4/Bi2MoO6复合粉体具有典型的纺锤形结构,长度约为2.5μm,宽度约为0.8μm。经实施例3制得的纺锤形BiVO4/Bi2MoO6复合粉体的紫外-可见漫反射(UV-vis DRS)谱图如图4中曲线(B)所示,表明所制备的复合样品的吸收边界为529nm。
对比例1:
步骤1. 在搅拌条件下,将V/Mo摩尔比为1:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即可得到对比例1中的BiVO4/Bi2MoO6复合粉体。
经对比例1制得的BiVO4/Bi2MoO6复合粉体的扫描电子显微镜(SEM)照片如图5所示,从图中可以看出,当V/Mo摩尔比为1:1时,所得BiVO4/Bi2MoO6复合粉体的形貌为杂乱无章的颗粒状,将不再是纺锤形结构。
Claims (1)
1.一种乙二醇诱导制备纺锤形BiVO4/Bi2MoO6复合粉体的水热-溶剂热法,其特征在于,包括以下步骤:
步骤1. 在搅拌条件下,将V/Mo摩尔比为2-4:1的偏钒酸铵和钼酸铵溶解于30mL热水(80℃)中,标记为A液;
步骤2. 在超声条件下,将8mmol硝酸铋溶解于30mL乙二醇中,标记为B液;
步骤3. 在室温搅拌条件下,将步骤1得到的A液逐滴加入步骤2得到的B液中,继续搅拌30min;
步骤4. 用2mol/L的NaOH溶液调节步骤3所得混合溶液的pH值为5,继续搅拌30min;
步骤5. 将步骤4得到的溶液转移至100mL反应釜内衬中,将密封好的反应釜置于恒温烘箱中于180℃下水热反应24h;
步骤6. 待自然冷却至室温后,取出样品对其进行抽滤,用去离子水和乙醇洗涤3次,将所得固体产物于60℃烘干12h,然后以5℃/min的升温速率升温到400℃,保温5h,即得到纺锤形BiVO4/Bi2MoO6复合粉体。
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