CN113231056B - 一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法 - Google Patents
一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,包括以下步骤:S1、将二水合氯化亚锡和硫脲混合溶解于去离子水中,在24‑27℃下搅拌12‑36h,得到二氧化锡量子点溶液;S2、取铌酸铵草酸盐水合物溶解于去离子水中,配置成铌浓度为0.2‑0.5mol/L的铌溶液;S3、将所得二氧化锡量子点溶液和铌溶液混合,在160‑180℃下进行水热法处理5‑7小时,得到铌掺杂二氧化锡量子点。本发明通过在二氧化锡量子点中掺杂铌,提高了光催化性能,在太阳光的作用下即可进行光催化,制备过程简单且成本低。
Description
技术领域
本发明属于量子点制备领域,具体涉及一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法。
背景技术
半导体光催化剂能利用半导体材料吸收外界辐射光能激发产生导带电子和价带空穴,进而与吸附在催化剂表面上的物质发生一系列化学反应。目前传统半导体光催化剂(如TiO2,ZnO等)存在光量子效率低、易失活和太阳能利用率不高等缺点,使得半导体光催化技术很难投入于实际应用中。因此,新型高效半导体光催化剂的研发成为当今光催化领域的研究热点。
二氧化锡(SnO2)作为一种光催化材料,具有稳定性好、成本低、制备简单等特点,并且对环境无毒无害,但SnO2的禁带宽度较宽,导致其对太阳光中的主要部分—可见光的吸收效率很低。目前,常采用掺杂、构建异质结等方法来缩小光催化材料的禁带宽度,以提高对可见光的利用率。然而现有的向光催化剂中掺杂银等金属的成本较高,难以实现大规模的应用。
发明内容
本发明针对以上问题的提出,而研究设计一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,来解决现有二氧化锡光催化材料的制备成本较高、可见光利用效率较低等问题。本发明采用的技术手段如下:
一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,包括以下步骤:
S1、将二水合氯化亚锡(SnCl2·2H2O)和硫脲(CH4N2S)混合溶解于去离子水中,在24-27℃下搅拌12-36h,得到二氧化锡量子点溶液;
S2、取铌酸铵草酸盐水合物(C2H2O4·x(NH3)·x(Nb))溶解于去离子水中,配置成铌浓度为0.2-0.5mol/L的铌溶液;
S3、将所得二氧化锡量子点溶液和铌溶液混合,在160-180℃下进行水热法处理5-7小时,得到铌掺杂二氧化锡量子点。
优选地,步骤S1中,二水合氯化亚锡和硫脲的质量比为(25-32):1。
优选地,步骤S1中,二氧化锡量子点溶液的浓度为0.17-0.22mol/L
优选地,步骤S1中,二氧化锡量子点溶液的浓度为0.2mol/L。
优选地,步骤S3中,铌掺杂二氧化锡量子点的粒径为3nm-8nm。
优选地,步骤S3中,二氧化锡量子点溶液与铌溶液的体积比为(23-24):1。
相较于SnO2光催化材料,SnO2量子点在其晶粒内部和表面都存在固有缺陷,表面上的缺陷可以作为吸附位点,用于吸附待催化材料。在光催化过程中,吸附在量子点表面的水分子与电子和空穴相互作用后产生高活性的羟基自由基,有效提高催化效率。并且SnO2量子点是一种无害环保材料,有无毒、化学稳定性好等优点。
与现有技术比较,本发明所述的一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法的有益效果为:
1、本发明以SnCl2·2H2O为主要原料,以CH4N2S作为催化剂,通过一步法在水溶液中制备了SnO2量子点,并通过掺杂Nb对量子点进行改性,制备的铌掺杂二氧化锡(Nb-SnO2)量子点具有优异的光催化性能。
2、本发明的Nb-SnO2量子点安全无污染,在实际应用的过程中,只需要在太阳光的作用下即可进行光催化,制备过程简单且成本低。
3、本发明的Nb-SnO2量子点在水溶液中具有长期稳定性,可以用于长期催化,并且能够重复利用。
附图说明
图1是本发明实施例制备的Nb-SnO2量子点的形貌图。
图2是本发明实施例制备的Nb-SnO2量子点的XRD图。
图3是O1s谱图的分峰拟合曲线。
图4是本发明实施例制备的Nb-SnO2量子点的紫外可见吸收光谱。
图5是Nb-SnO2量子点的禁带宽度估算。
图6是XPS价带谱图。
图7是Nb-SnO2量子点的能带结构。
图8为不同辐射光源下Nb-SnO2量子点对聚乙烯膜的催化降解率。
具体实施方式
一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,包括以下步骤:
S1、将二水合氯化亚锡(SnCl2·2H2O)和硫脲(CH4N2S)混合溶解于去离子水中,在24℃-27℃下搅拌12-36h,得到二氧化锡量子点溶液;
S2、取铌酸铵草酸盐水合物(C2H2O4·x(NH3)·x(Nb))溶解于去离子水中,配置成铌浓度为0.2-0.5mol/L的铌溶液;
S3、将所得二氧化锡量子点溶液和铌溶液混合,在160-180℃下进行水热法处理5-7小时,得到铌掺杂二氧化锡量子点。
优选地,步骤S1中,二水合氯化亚锡和硫脲的质量比为(25-32):1,二氧化锡量子点溶液的浓度为0.17-0.22mol/L。步骤S3中,铌掺杂二氧化锡量子点的粒径为3nm-8nm,二氧化锡量子点溶液与铌溶液的体积比为(23-24):1。
本发明提供的简单、廉价、环保的二氧化锡量子点合成方法,具体包括以下步骤:
(1)分别称取2.257g二水合氯化亚锡(SnCl2·2H2O)和0.077g硫脲(CH4N2S);
(2)将上述两种物质混合溶解于50ml去离子水中,在磁搅拌装置中25℃下水浴搅拌24h,在SnCl2水解氧化后,得到了水性SnO2量子点溶液;
(3)将1g铌酸铵草酸盐水合物(C2H2O4·x(NH3)·x(Nb))溶解于10ml去离子水中,得到铌溶液;
(4)取0.425ml步骤(3)中所得铌溶液和10ml步骤(2)中所得SnO2量子点水溶液,混合后放入聚四氟乙烯(也可以用PPL等其它材质,只要耐高温即可)水热釜中,在160℃下进行6小时的水热法处理,得到Nb-SnO2量子点。
对所得Nb-SnO2量子点进行性能检测,结果如图1-8。
图1是用高分辨率透射电镜(HRTEM)观察的本发明制备的Nb-SnO2量子点的形貌,可见量子点间没有明显团聚,表现出良好的分散性和均匀性。由图中可以看出,Nb-SnO2量子点的特征间距为0.321-0.325nm,对应于SnO2晶格的(110)面,并且Nb-SnO2量子点在水溶液中具有均匀的分散性,量子点平均晶粒尺寸为5.6nm左右。
图2为本发明制备的Nb-SnO2量子点的X射线衍射图样与标准SnO2样品衍射峰,由图中可以看出,在26.5°、33.9°、38.2°、51.7°有四个主峰,分别对应(110)、(200)、(101)和(211)晶面,与标准图谱一致。通过计算表明,SnO2晶胞的晶格参数为和/>根据Scherrer公式,晶粒的平均晶粒尺寸的计算结果为5.3nm。
图3是O1s谱图的分峰拟合曲线,其是利用高斯-洛伦兹函数拟合和分峰。图中在531.76eV和530.97eV处得到两个子峰,分别对应于氧原子的两个化学态。O(I)峰,中心为531.76eV,表示与Sn原子完全配位的氧原子。O(II)峰中心为530.97eV,结合能比O(I)低0.79eV。它是由Sn和O原子之间的非化学计量配位引起的,可推断出氧空位的存在,而氧空位是SnO2材料的固有缺陷。
图4是所制备的Nb-SnO2量子点的紫外可见吸收光谱(UV-Vis光谱),根据该紫外-可见光谱,运用Tauc Plot法计算可以得到其禁带宽度。
图5是禁带宽度估算,通过(αhν)2对hν的线性拟合外推图,计算得出禁带宽度Eg值为2.95eV。
图6是XPS价带谱图,通过XPS价带谱测算价带顶位置,得价带顶位于3.58eV,根据EC=EV-Eg,可以计算出导带底的位置为0.63eV。
图7是Nb-SnO2量子点的能带结构,其中Ev为3.58eV,高于水氧化为超氧自由基的能量。
图8所示为制备的Nb-SnO2量子点在不同辐射光源照射下对聚乙烯膜降解率的影响,在紫外光和可见光的照射下,Nb-SnO2量子点对聚乙烯膜均有明显的光催化降解效率。并且紫外光由于具有更高的光子能量,可以激发出更多的光生电子空穴对,其光催化效率相对更高。
本发明中通过对间隔20天的光催化剂进行XRD、XPS检测,显示量子点结构无明显差别,可见本发明的Nb-SnO2量子点在20天的时间内表现出的电性能和降解效率并无较大差距,表明本发明的Nb-SnO2量子点在水溶液中具有长期稳定性,可以用于长期催化,并且能够重复利用。
以上所述的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (5)
1.一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,其特征在于:包括以下步骤:
S1、将二水合氯化亚锡和硫脲混合溶解于去离子水中,在24-27℃下搅拌12-36h,得到二氧化锡量子点溶液;
S2、将1g铌酸铵草酸盐水合物(C2H2O4·x(NH3)·x(Nb))溶解于10ml去离子水中,得到铌溶液;
S3、取0.425ml步骤S2中所得铌溶液和10ml步骤S1中所得SnO2量子点水溶液,混合后放入水热釜中,在160℃下进行6小时的水热法处理,得到Nb-SnO2量子点。
2.根据权利要求1所述的一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,其特征在于:步骤S1中,二水合氯化亚锡和硫脲的质量比为(25-32):1。
3.根据权利要求1所述的一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,其特征在于:步骤S1中,二氧化锡量子点溶液的浓度为0.17-0.22mol/L。
4.根据权利要求3所述的一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,其特征在于:步骤S1中,二氧化锡量子点溶液的浓度为0.2mol/L。
5.根据权利要求1所述的一种铌掺杂改性二氧化锡量子点可见光催化材料的制备方法,其特征在于:步骤S3中,铌掺杂二氧化锡量子点的粒径为3-8nm。
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