CN108262035B - 一种机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法 - Google Patents
一种机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法 Download PDFInfo
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Abstract
本发明公开了一种机械球磨热处理两步法合成三氧化二铋‑二氧化铈纳米复合物的方法,其是将固相原料二水合铋酸钠、亚硫酸氢钠和五水合硝酸铈混合后,进行机械球磨固相反应,获得BiONO3‑CeO2前驱体,对所述BiONO3‑CeO2前驱体进行热处理,即制得目标产物Bi2O3‑CeO2纳米复合物。本发明采用固体混合,原料室温球磨固相反应和热处理两步法,制备过程简单,易于控制并能大量减少产物粒子的团聚;避免另外添加氧化还原剂、模板剂和溶剂,提高了产物纯度,符合材料绿色化合成的要求,也适合于大规模生产。
Description
技术领域
本发明属于纳米材料及其制备领域,特别涉及一种Bi2O3/CeO2纳米复合物的制备方法。
背景技术
Bi2O3是一种重要的氧化物半导体材料,由于其具有较低的带隙能,可以吸收可见光,能被可见光激发,具有可见光光催化性能,成为太阳能光催化降解环境污染物的一种很有应用潜力的光催化材料。但是,单一的Bi2O3半导体,在光的照射下,其光生载流子容易复合,导致光量子效率降低,影响光催化效率。为了提高光生载流子的分离,延长生载流子的寿命,提高光催化效率,可以对Bi2O3半导体进行改性,将Bi2O3与能带匹配的半导体进行复合将是一种有效的改性方法。众所周知,CeO2是一种重要的氧化物半导体功能材料,其具有和Bi2O3匹配的能带结构,可以预见Bi2O3/CeO2纳米复合物将具有优越的可见光光催化性能,在太阳能光催化降解环境污染物方面将具有广阔的应用前景。
目前,Bi2O3基纳米复合物的主要制备方法是液相法制备方法。比如:Sood等人以Bi(NO3)3·5H2O和钛酸丁酯为原料,通过水热反应的方法制备出Bi2O3/TiO2异质结光催化剂(S.Sood et al.Chemical Engineering Journal,2016,290:45–52.);Xu等人以Bi2O3粉和钛酸丁酯为原料,采用溶胶-凝胶的方法制备出Bi2O3/TiO2复合粒子(J.-J.Xu etal.Chemical Engineering Journal,2016,290:45–52.);Wang等人以Bi(NO3)3·5H2O和氧化石墨烯为原料,采用水热和煅烧两步法制备出Bi2O3/Graphene纳米复合物(H.-W.Wang etal.Electrochimica Acta,2010,55:8974–8980.),等等。
现有的制备方法虽然可以制备出Bi2O3基复合材料,但仍然存在一些不足,比如:液相法制备的产物粒子容易发生团聚,降低产品性能;有的在制备过程中需要使用大量有机溶剂,带来环境污染;有的制备过程复杂且成本高,不利于大规模生产。所以,有待于进一步探索开发成本低、过程简单、易于大规模生产的新制备方法。
发明内容
本发明的目的在于克服现有技术的不足,提供一种工艺简单、操作方便的室温机械球磨和热处理两步法制备Bi2O3/CeO2纳米复合物的方法。
为实现发明目的,本发明采用如下技术方案:
本发明机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法,其特点在于:将固相原料二水合铋酸钠、亚硫酸氢钠和五水合硝酸铈混合后,进行机械球磨固相反应,获得BiONO3-CeO2前驱体,对所述BiONO3-CeO2前驱体进行热处理,然后再经洗涤、离心分离及干燥后,即制得目标产物Bi2O3-CeO2纳米复合物。
其中:所述二水合铋酸钠、亚硫酸氢钠和五水合硝酸铈的摩尔比为2:1.5:1。所述机械球磨固相反应是指:将混合后原料放入氧化锆球磨罐中,再置于球磨机中,设定转速480rpm,球磨反应6小时。所述热处理是将BiONO3-CeO2前驱体在400℃下加热2~10小时。所述洗涤是用蒸馏水进行洗涤,所述干燥是在60℃、0.1Mpa真空度下真空干燥2小时。
如下式所示:本发明在室温下通过对二水合铋酸钠(NaBiO3·2H2O)、亚硫酸氢钠(NaHSO3)和五水合硝酸铈(Ce(NO3)3·5H2O)固体混合原料的机械球磨而引发固相反应,制备出纳米BiONO3-CeO2前驱体。BiONO3-CeO2前驱体在一定温度下加热处理一定时间,获得Bi2O3/CeO2纳米复合物,从而实现本发明的目的。
与现有技术相比,本发明的有益效果体现在:
1、本发明提供的固体混合反应原料的室温固相球磨反应制备技术,制备过程简单、易于控制并减少产物粒子的团聚;
2、本发明提供的Bi2O3/CeO2纳米复合物的制备方法,不需要使用溶剂,除固体原料外不额外添加任何氧化还原剂、模板剂、表面活性剂,提高了产物纯度,也符合材料绿色化合成的要求;
3、本发明提供的Bi2O3/CeO2纳米复合物的制备方法,工艺简单、操作安全可靠、易于工业化生产。
附图说明
图1为本发明实施例1、2、3制备的产物的XRD图谱;
图2为本发明实施例3所制备产物的TEM图像。
具体实施方式
下面结合附图对本发明的实施例作详细说明,下述实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
按照2:1.5:1的摩尔比称取0.02摩尔二水合铋酸钠、0.015摩尔亚硫酸氢钠和0.01摩尔五水合硝酸铈加入配备50个直径6mm氧化锆磨球和8个直径10mm氧化锆磨球的50mL氧化锆球磨罐中,在QM-3SP04行星式高能球磨机中于480rpm下连续球磨6小时后,将球磨反应所得产物在400℃下煅烧2小时并冷却至室温,随后用蒸馏水对产物进行洗涤,离心分离并在60℃、0.1Mpa真空度下真空干燥2小时,得到目标产物。
实施例2
按照2:1.5:1的摩尔比称取0.02摩尔二水合铋酸钠、0.015摩尔亚硫酸氢钠和0.01摩尔五水合硝酸铈加入配备50个直径6mm氧化锆磨球和8个直径10mm氧化锆磨球的50mL氧化锆球磨罐中,在QM-3SP04行星式高能球磨机中于480rpm下连续球磨6小时后,将球磨反应所得产物在400℃下煅烧4小时并冷却至室温,随后用蒸馏水对产物进行洗涤,离心分离并在60℃、0.1Mpa真空度下真空干燥2小时,得到目标产物。
实施例3
按照2:1.5:1的摩尔比称取0.02摩尔二水合铋酸钠、0.015摩尔亚硫酸氢钠和0.01摩尔五水合硝酸铈加入配备50个直径6mm氧化锆磨球和8个直径10mm氧化锆磨球的50mL氧化锆球磨罐中,在QM-3SP04行星式高能球磨机中于480rpm下连续球磨6小时后,将球磨反应所得产物在400℃下煅烧10小时并冷却至室温,随后用蒸馏水对产物进行洗涤,离心分离并在60℃、0.1Mpa真空度下真空干燥2小时,得到目标产物。
上述实施例所得目标产物的X-射线衍射分析(XRD分析):分别将实施例1、2和3制得的目标产物进行XRD分析,结果见图1,可以看出,在XRD图谱中只有Bi2O3和CeO2特征衍射峰,没有其它物相的衍射峰存在,表明球磨6小时后,铋酸钠与亚硫酸氢钠和硝酸铈固相反应完全。
由Scherrer公式计算得到:反应原料二水合铋酸钠亚硫酸氢钠和五水合硝酸铈按照2:1.5:1的摩尔比混合后并连续球磨6小时后,将球磨反应所得产物在400℃下分别煅烧2小时、4小时、10小时后,所得复合产物Bi2O3/CeO2中(Bi2O3、CeO2)的平均晶粒尺寸分别为(32.2nm、19.3nm)、(37.7nm、21.5nm)、(42.9nm、29.8nm),表明随着加热时间的延长,产物中Bi2O3和CeO2的平均晶粒尺寸逐渐增大。在制备过程中,可以通过适当改变加热时间来控制复合产物中Bi2O3和CeO2的平均晶粒尺寸。
上述实施例3所得产物的透射电子显微镜观察(TEM图像):将实施例3制得的产物进行透射电子显微镜观察,其图像见图2。从图像可以看出,实施例3制得的产物颗粒大小大约为30-45nm,粒子之间有明显的异质结存在。
本领域普通技术人员可以理解:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (3)
1.一种机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法,其特征在于:将固相原料二水合铋酸钠、亚硫酸氢钠和五水合硝酸铈混合后,进行机械球磨固相反应,获得BiONO3-CeO2前驱体,对所述BiONO3-CeO2前驱体进行热处理,然后再经洗涤、离心分离及干燥后,即制得目标产物Bi2O3-CeO2纳米复合物;
所述机械球磨固相反应是指:将混合后原料放入氧化锆球磨罐中,再置于球磨机中,设定转速480rpm,球磨反应6小时;
所述热处理是将BiONO3-CeO2前驱体在400℃下加热2~10小时。
2.根据权利要求1所述的机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法,其特征在于:所述二水合铋酸钠、亚硫酸氢钠和五水合硝酸铈的摩尔比为2:1.5:1。
3.根据权利要求1所述的机械球磨热处理两步法合成三氧化二铋-二氧化铈纳米复合物的方法,其特征在于:所述洗涤是用蒸馏水进行洗涤,所述干燥是在60℃、0.1Mpa真空度下真空干燥2小时。
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