CN110479265A - 一种稀土掺杂纳米压电催化剂的制备方法 - Google Patents
一种稀土掺杂纳米压电催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种稀土掺杂纳米压电催化剂的制备方法。称取预定量的钛酸铋钾原料以及稀土离子氧化物以及添加剂,置于强碱溶液中进行磁力搅拌,而后转移到水热反应釜中进行水热反应,本发明通过水热法制备出的Ag2O修饰稀土掺杂的钛酸铋钾压电催化剂,制备工艺简便,本发明方法是通过水热法一步合成,只需控制相关反应条件,操作方法简单且成熟;结晶度好杂质少,通过水热法一步合成Ag2O修饰稀土掺杂的钛酸铋钾,所制备出的掺杂后的钙钛矿陶瓷粉末的结晶度十分优异,杂质少;制备得到的钛酸铋钾纳米颗粒具有良好的压电催化性能。
Description
技术领域
本发明属于低维纳米材料制备领域,特别涉及一种稀土掺杂纳米压电催化剂的制备方法。
背景技术
近年科研学者对钙钛矿结构材料的研究日益加深,成为了材料界冉冉升起的一颗明星,具有着无穷的魅力。在钙钛矿结构中由于存在一个宽容系数t,故其可以很好的掺杂入各类离子尺寸不同的元素引起畸变,而不改变典型的钙钛矿结构,在标准宽容系数范围的以外的才会变化晶体结构形成新的相。理想情况下,宽容系数t被定义为:
其中rA、rB、rO分别表示A、B、O位离子的离子半径,t=1时材料晶体结构为紧密堆积,理论上t的区间范围为0.9~1.1。
钛酸铋钾(K0.5Bi0.5TiO3,简称BKT)是在钛酸铋钠之后发展起来的压电材料。在298K下,其晶体结构是四方钙钛矿,具有比钛酸铋钠(简称BNT)高的居里温度(Tc=380℃),因此很有希望成为新一代高温压电器件所用的压电陶瓷材料。
催化剂在生活中的应用是多方面的,比如水分解,原油裂解,污水处理,染料降解等。由于压电材料独特的压电性能在,在力的作用面上会产生正负电荷的积累。正电荷具有氧化的能力,负电荷具有了还原能力,这样压电材料在形变的情况下就具有了氧化还原的能力可以很好的运用于催化有机物的分解。简而言之,压电材料在外界机械振动下本身会发生受迫振动而产生形变进而在表面上形成正负电荷,对有机物进行分解。相比于光催化剂的广泛研究,人们对于掺杂稀土的压电催化剂的研究还需更进一步加强。因此本发明设计了一种新的制备工艺简便、结晶度好杂质少、具有良好的压电催化性能的稀土掺杂纳米压电催化剂的制备方法。
发明内容
为了解决现有技术中存在的上述技术问题,本发明提供了一种稀土掺杂纳米压电催化剂的制备方法,本发明采用如下技术方案:
一种稀土掺杂纳米压电催化剂的制备方法,包括如下步骤:
(a)根据化学计量比称取预定量的钛酸铋钾原料、预定量的稀土离子氧化物以及预定量的添加剂,置于强碱溶液中进行磁力搅拌。
(b)将搅拌混合之后的悬浊液倒入到聚四氟乙烯反应釜内套中,将封闭好的反应釜内套置于不锈钢外套中,螺丝拧紧。
(c)将拧紧的整个水热反应釜置于烘箱中保温。
(d)将保温结束后样品放置于离心管中用离心机进行离心清洗。
(e)将离心清洗得到的样品烘干后得到催化剂。
作为优选,所述步骤(a)所用原料除铋源是硝酸盐外都是氧化物,所述添加剂为AgNO3,其Ag元素质量百分比为:1%~3%,稀土离子氧化物掺杂的摩尔百分比为:0.01%-1%;所述强碱溶液为KOH溶液,其浓度为10mol/L~12mol/L。
作为优选,所述钛酸铋钾原料包括硝酸铋、氧化钛和碳酸钾,所述稀土离子氧化物包括氧化铒、氧化镱中的至少一种。
作为优选,所述步骤(c)中温度制度为:从室温升至保温时间的升温速率为:1℃/min~5℃/min;保温温度为:180℃~220℃;保温时间为:24-48h;炉冷。
作为优选,所述步骤(d)中离心机的转速速率为2000r/min~20000r/min。
作为优选,所述步骤(e)中样品烘干温度为:80℃-120℃。
本发明通过水热法制备出的Ag2O修饰稀土掺杂的钛酸铋钾压电催化剂具有如下优点:
1.制备工艺简便,本发明方法是通过水热法一步合成,只需控制相关反应条件,操作方法简单且成熟;
2.结晶度好杂质少。本方法是通过水热法一步合成Ag2O修饰稀土掺杂的钛酸铋钾,所制备出的掺杂后的钙钛矿陶瓷粉末的结晶度十分优异,杂质少;
3.制备得到的钛酸铋钾纳米颗粒具有良好的压电催化性能。
附图说明
图1是本发明所制备的稀土掺杂钛酸铋钾的XRD图谱;
图2是本发明所制备纳米材料的激光粒度分析图;
图3是本发明所制备纳米材料在催化罗丹明溶液的紫外可见吸收光谱;
具体实施方式
下面结合附图对本发明做进一步的描述,通过下面对实施例的描述,将更加有助于公众理解本发明,但不能也不应当将申请人所给出的具体的实施例视为对本发明技术方案的限制,任何术特征的定义进行改变或对整体结构作形式的而非实质的变换都应视为本发明的技术方案所限定的保护范围。
实施例1
一种稀土掺杂纳米压电催化剂的制备方法,包括如下步骤:
步骤a,称取2.44985g硝酸铋、0.01926g氧化铒、0.01970g氧化镱、0.79667g氧化钛、0.34902g碳酸钾以及0.06491g硝酸银粉末,放入到盛有12mol/L KOH溶液中磁力搅拌20min。
步骤b,将搅拌混合之后的悬浊液倒入到聚四氟乙烯反应釜内套中,将封闭好的反应釜内套置于不锈钢外套中,螺丝拧紧。
步骤c,将整个水热反应釜放于高温烘箱中,设置温度制度为:从室温以3℃/min的升温速率升至200℃并保温24小时,而后随炉冷却至室温后取出。
步骤d,打开反应釜将上层清液倒入废液桶中,将沉淀物取出放到离心管中。依次加入乙醇和水,进行一次离心乙醇洗,两次离心水洗。离心机的设置为:以8000r/min的离心速率洗涤样品5min。
步骤e,在100℃烘箱中进行干燥。
步骤f,取出干燥后的样品进行研磨,得到细粉样催化剂。
本是实例中:如图1是稀土掺杂钛酸铋钾的XRD图谱,对照K0.5Bi0.5TiO3的X射线标准衍射图谱,可以得出,本方法制备的产物主要成分为K0.5Bi0.5TiO3,以及部分的铒离子化合物、镱离子化合物,表明本方法通过水热法一步合成Ag2O修饰稀土掺杂的钛酸铋钾,所制的结晶度好杂质少。
如图2是本发明所制备纳米材料的激光粒度分析图,由图可得,本产物的粒子粒径约为62~256nm;
如图3是本发明所制备纳米材料在催化罗丹明溶液的紫外可见吸收光谱;
实施例2
一种稀土掺杂纳米压电催化剂的制备方法,包括如下步骤:
步骤a,称取2.44985g硝酸铋、0.01926g氧化铒、0.01970g氧化镱、0.79667g氧化钛、0.34902g碳酸钾以及0.06491g硝酸银粉末,放入到盛有10mol/L KOH溶液中磁力搅拌20min。
步骤b,将搅拌混合之后的悬浊液倒入到聚四氟乙烯反应釜内套中,将封闭好的反应釜内套置于不锈钢外套中,螺丝拧紧。
步骤c,将整个水热反应釜放于高温烘箱中,设置温度制度为:从室温以2℃/min的升温速率升至190℃并保温36小时,而后随炉冷却至室温后取出。
步骤d,打开反应釜将上层清液倒入废液桶中,将沉淀物取出放到离心管中。依次加入乙醇和水,进行一次离心乙醇洗,两次离心水洗。离心机的设置为:以10000r/min的离心速率洗涤样品5min。
步骤e,在90℃烘箱中进行干燥。
步骤f,取出干燥后的样品进行研磨,得到细粉样催化剂。
实施例3
一种稀土掺杂纳米压电催化剂的制备方法,包括如下步骤:
步骤a,称取2.44985g硝酸铋、0.01926g氧化铒、0.01970g氧化镱、0.79667g氧化钛、0.34902g碳酸钾以及0.06491g硝酸银粉末,放入到盛有11mol/L KOH溶液中磁力搅拌20min。
步骤b,将搅拌混合之后的悬浊液倒入到聚四氟乙烯反应釜内套中,将封闭好的反应釜内套置于不锈钢外套中,螺丝拧紧。
步骤c,将整个水热反应釜放于高温烘箱中,设置温度制度为:从室温以1℃/min的升温速率升至220℃并保温18小时,而后随炉冷却至室温后取出。
步骤d,打开反应釜将上层清液倒入废液桶中,将沉淀物取出放到离心管中。依次加入乙醇和水,进行一次离心乙醇洗,两次离心水洗。离心机的设置为:以12000r/min的离心速率洗涤样品5min。
步骤e,在120℃烘箱中进行干燥。
步骤f,取出干燥后的样品进行研磨,得到细粉样催化剂。
以上所述方案,仅仅是本发明的几种水热法合成Ag2O表面修饰的稀土掺杂压电材料的较佳实施例而已,并非对本发明的保护范围产生任何限制。
本发明通过水热法制备出的Ag2O修饰稀土掺杂的钛酸铋钾压电催化剂,制备工艺简便,本发明方法是通过水热法一步合成,只需控制相关反应条件,操作方法简单且成熟;结晶度好杂质少,通过水热法一步合成Ag2O修饰稀土掺杂的钛酸铋钾,所制备出的掺杂后的钙钛矿陶瓷粉末的结晶度十分优异,杂质少;制备得到的钛酸铋钾纳米颗粒具有良好的压电催化性能。
当然,本发明还可以有其他多种实施例,在不背离本发明精神及其实质的情况下,熟悉本领域的技术人员可以根据本发明做出各种相应的改变和变形,但这些相应的改变和变形都应属于本发明所附的权利要求的保护范围。
Claims (6)
1.一种稀土掺杂纳米压电催化剂的制备方法,其特征在于,包括如下步骤:
(a)根据化学计量比称取预定量的钛酸铋钾原料、预定量的稀土离子氧化物以及预定量的添加剂,置于强碱溶液中进行磁力搅拌;
(b)将搅拌混合之后的悬浊液倒入到聚四氟乙烯反应釜内套中,将封闭好的反应釜内套置于不锈钢外套中,螺丝拧紧;
(c)将拧紧的整个水热反应釜置于烘箱中保温;
(d)将保温结束后样品放置于离心管中用离心机进行离心清洗;
(e)将离心清洗得到的样品烘干后得到催化剂。
2.根据权利要求1所述的一种稀土掺杂纳米压电催化剂的制备方法,其特征在于:所述步骤(a)所用原料除铋源是硝酸盐外都是氧化物,所述添加剂为AgNO3,其Ag元素质量百分比为:1%~3%,稀土离子氧化物掺杂的摩尔百分比为:0.01%-1%;所述强碱溶液为KOH溶液,其浓度为10mol/L~12mol/L。
3.根据权利要求1所述一种稀土掺杂压电催化纳米材料的制备方法,其特征在于:所述钛酸铋钾原料包括硝酸铋、氧化钛和碳酸钾,所述稀土离子氧化物包括氧化铒、氧化镱中的至少一种。
4.根据权利要求1所述的一种稀土掺杂纳米压电催化剂的制备方法,其特征在于:所述步骤(c)中温度制度为:从室温升至保温时间的升温速率为:1℃/min~5℃/min;保温温度为:180℃~220℃;保温时间为:24-48h。
5.根据权利要求1所述的一种稀土掺杂纳米压电催化剂的制备方法,其特征在于:所述步骤(d)中离心机的转速速率为2000r/min~20000r/min。
6.根据权利要求1所述一种稀土掺杂压电催化纳米材料的制备方法,其特征在于:所述步骤(e)中样品烘干温度为:80℃-120℃。
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