CN104480429B - 一种铂纳米颗粒负载介孔氧化铝原位制备方法 - Google Patents
一种铂纳米颗粒负载介孔氧化铝原位制备方法 Download PDFInfo
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Abstract
本发明属于纳米材料技术领域,是一种利用磁控溅射和阳极氧化双联技术原位制备铂纳米颗粒负载介孔氧化铝的方法。本发明的目的是提供一种工序简单、成本低、纳米颗粒分散性好且不易团聚的铂纳米颗粒负载介孔氧化铝生产方法。本发明的技术方案是一种铂纳米颗粒负载介孔氧化铝原位制备方法,包括Al‑Pt二元合金的制备及阳极氧化两个步骤。采用本发明方法制备铂纳米颗粒负载介孔氧化铝具有工序简单、成本低、纳米颗粒分散性好、纳米颗粒不易团聚等特点。
Description
技术领域
本发明属于纳米材料技术领域,是一种利用磁控溅射和阳极氧化双联技术原位制备铂纳米颗粒负载介孔氧化铝的方法。
背景技术
介孔材料(Mesoporous material)一般指孔径分布在2-50nm的多孔材料。由于介孔材料在催化剂、离子交换、传感器等领域有广阔的应用前景而受到材料研究者的关注。然而介孔材料的这些应用均要依赖于介孔材料本身所不具有的一些特殊性能。通过在介孔材料中引入具有特殊功能的纳米颗粒即可实现介孔材料的特殊性能,比如在催化剂领域里应用的Pd、Pt纳米颗粒、在磁性材料领域应用的Fe及其氧化物颗粒、在光学领域应用的Ag-Au合金颗粒等。然而,要想将纳米颗粒均匀的分散到介孔材料里面,同时保证其在后续的生产和使用过程中不发生团聚和长大仍然是一项巨大的挑战。
传统制备纳米颗粒负载介孔氧化物复合结构的方法主要包括介孔氧化物的制备和纳米颗粒的加载两个过程。介孔氧化物的制备又有氧化还原法、溶胶-凝胶法、阳极氧化法等,总体上比较成熟。而纳米颗粒的加载工艺复杂、技术要求高、控制难度大,是制备过程的成本和质量控制步骤。纳米颗粒的加载一般通过化学/电化学沉积的方法来完成,即将制备好的介孔氧化物载体浸在含有要加载的金属或金属离子的溶液中,通过化学/电化学沉积制得纳米金属颗粒,然后再进行干燥得到纳米颗粒负载介孔氧化物。目前,传统制备纳米颗粒负载介孔氧化物的工艺仍然面临纳米金属颗粒的分散度不够高以及纳米金属颗粒在制备和使用过程中容易团聚两个突出问题。
发明内容
本发明的目的是提供一种工序简单、成本低、纳米颗粒分散性好且不易团聚和长大的铂纳米颗粒负载介孔氧化铝生产方法。
本发明的技术方案是一种铂纳米颗粒负载介孔氧化铝原位制备方法,包括如下步骤:
a、制备Al-Pt二元合金:在直径为5cm的纯铝靶材上缠绕2~5根直径0.5~1mm、长3~5cm的铂丝制成Al-Pt复合靶材;以铝片为基材,通过Al-Pt复合靶材和纯Al靶材双靶共溅射的方法制备Al-Pt二元合金;溅射电流分别为Al-Pt复合靶材110~200mA和纯Al靶200~320mA;溅射时间为10~20min;
b、阳极氧化:将步骤a获得的Al-Pt二元合金置于0.3~0.6M的硫酸水溶液中,在0~6V动电位或恒电位阳极氧化,制备出铂纳米颗粒负载介孔氧化铝。
具体的,步骤a中在铝基材上获得一层厚100~200nm的Al-Pt二元合金,铂含量为1at%~5at%。
具体的,步骤b中在Al-Pt二元合金上制备出一层厚100~200nm的铂纳米颗负载介孔氧化铝,铂纳米颗粒的尺寸为5~50nm,且均匀弥散的分布于介孔氧化铝的孔壁之中。
具体的,步骤a中,溅射电流分别为Al-Pt复合靶材110mA和纯Al靶320mA;溅射时间为10min。
具体的,步骤b中硫酸水溶液浓度为0.4M。
具体的,步骤b中在3V电压阳极氧化20min。
本发明的有益效果:
本发明方法中介孔氧化物的制备和金属纳米颗粒的加载不是分开而是同步进行,所以生产工序更加简便;金属纳米颗粒随氧化膜孔的形成而分散,所以分散度更高且易于控制;金属纳米颗粒之间有氧化膜物质存在,可防止纳米颗粒在使用过程中(尤其在高温条件下)的烧结和团聚;本工艺的关键步骤为磁控溅射和阳极氧化两个传统技术,具有技术容易掌握、投资成本低等特点,因此利于后期的技术推广和应用。本发明方法是对传统阳极氧化技术的创造性发展,在化学催化、离子交换、传感器等领域有广阔的应用前景,同时对开发其它金属颗粒负载介孔氧化物功能材料有重要的启发意义。
附图说明
图1:磁控溅射获得的Al-Pt二元合金表面形貌
图2:磁控溅射获得的Al-Pt二元合金截面形貌
图3:0-6V动电位阳极氧化获得的铂纳米颗粒负载介孔氧化铝的表面形貌
图4:0-6V动电位阳极氧化获得的铂纳米颗粒负载介孔氧化铝的截面形貌
图5:3V恒压阳极氧化20min得到的铂纳米颗粒负载介孔氧化铝表面形貌
图6:3V恒压阳极氧化20min得到的铂纳米颗粒负载介孔氧化铝截面形貌
具体实施方式
本发明为了克服传统工艺的缺点,将介孔材料的制备和纳米颗粒的加载两个过程同时完成。研究表明,在阳极氧化Al、Ti、Zr等阀金属为基的合金时,如果固溶体合金中所包含的合金元素对应的氧化物生成吉布斯自由能变(△G0)比阀金属氧化物的△G0更正,那么合金元素将首先在金属表面富集,然后取决于加载电压和△G0值的大小,要么发生氧化,要么以金属纳米颗粒的形式进入多孔阳极氧化膜结构中。因此,如果可以设法得到A-B二元合金,其中A为介孔氧化物的金属源(如Al、Ti、Zr等),B为纳米金属颗粒的金属源(如Pt、Au、Ag等),然后将该二元合金在酸性溶液中进行阳极氧化,通过控制二元合金的成分(惰性元素含量过多时阳极氧化难以进行)和阳极氧化条件(惰性元素的稳定性越强发生选择性氧化的电压范围越大),就有望通过一步法获得纳米颗粒负载介孔氧化物。这正是本发明专利的理论依据。
本发明中,通过控制Al-Pt复合靶材及纯Al靶材的溅射电流来控制Al-Pt二元合金中Al︰Pt的比例;通过控制阳极氧化电压及加载方式控制介孔氧化铝的孔隙度及铂纳米颗粒的尺寸和分散程度。
实施例1
a、制备Al-Pt二元合金
(1)取直径0.5mm的铂丝216mm,分5段固定在直径50mm的纯Al靶材上,制成Al-Pt复合靶材;
(2)取另外一个直径为50mm纯Al靶材作为第二靶材;
(3)将两个靶材装入样品仓内,设定纯Al靶材溅射电流为320mA、Al-Pt复合靶材的溅射电流为110mA,磁控溅射时间为10min,在纯铝基材上溅射一层Al-Pt二元合金;
(4)采用场发射扫描电镜观察Al-Pt二元合金的表面形貌,如图1所示;
(5)采用显微切割技术制备透射电镜样品(样品名义厚度15nm),然后在透射电镜上进行组织观察,如图2所示,其中Al-Pt二元合金的厚度约为145nm,成分(原子百分比)为98.35%Al,1.65%Pt。
b、阳极氧化Al-Pt二元合金
(1)取浓度为98.3%的浓硫酸(密度为1.84g/cm3)0.22ml,缓慢加入到适量去离子水中,配制成浓度为0.4M的硫酸水溶液;
(2)取步骤a中制备的沉积有Al-Pt二元合金的铝片,将样品的边缘和背面用有机漆进行封闭,留出面积为1cm2的Al-Pt二元合金表面,冷风干燥待用;
(3)在恒电位仪上进行阳极氧化:将封闭好的样品放入配制好的硫酸水溶液中并与电源的正极相连;将电源的负极与环形的纯铝片相连;采用饱和甘汞电极为参比电极;从开路电位(OCP)开始正向扫描至6V(OCP),扫描速率为33mv/s,制备出铂纳米颗粒负载介孔氧化铝;
(4)采用场发射扫描电镜观察铂纳米颗粒负载介孔氧化铝的表面形貌,如图3所示,其中微孔的大小为10-25nm;
(5)采用纳米显微切割技术制备透射电镜样品(样品名义厚度15nm),然后在透射电子显微镜上进行组织观察,铂纳米颗粒负载介孔氧化铝的组织如图4所示,其中铂纳米颗粒负载介孔氧化铝的厚度约为100nm,铂纳米颗粒(黑色点)的大小为3-20nm。
实施例2
a、制备Al-Pt二元合金
Al-Pt二元合金的制备过程同实施例1中的a步骤。
b、制备铂纳米颗粒负载介孔氧化铝
(1)同实施例1中的b步骤中的(1)。
(2)同实施例1中的b步骤中的(2)。
(3)在恒电位仪上进行阳极氧化:将封闭好的样品放入配制好的硫酸水溶液中并与电源的正极相连;将电源的负极与环形的纯铝片相连;采用饱和甘汞电极为参比电极;在恒定电位3V(OCP)下进行阳极氧化20min,制备出铂纳米颗粒负载介孔氧化铝。
(4)采用场发射扫描电镜观察铂纳米颗粒负载介孔氧化铝的表面形貌,如图5所示,其中微孔大小为9-20nm;
(5)采用纳米显微切割技术制备透射电镜样品(样品名义厚度15nm),然后在透射电子显微镜上进行组织观察,如图6所示,其中铂纳米颗粒负载介孔氧化铝的厚度约为150nm,铂纳米颗粒(黑色点)的大小为5-15nm。
实施例3
a、制备Al-Pt二元合金
(1)取直径1mm的铂丝95mm,分2段固定在直径50mm的纯Al靶材上,制成Al-Pt复合靶材;
(2)取另外一个直径为50mm纯Al靶材作为第二靶材;
(3)将两个靶材装入样品仓内,设定纯Al靶材溅射电流为200mA、Al-Pt复合靶材的溅射电流为200mA,磁控溅射时间为15min,在纯铝基材上溅射一层Al-Pt二元合金,其中Al-Pt二元合金的厚度约为165nm,成分(原子百分比)为96.5%Al,3.5%Pt。
b、阳极氧化Al-Pt二元合金
(1)取浓度为98.3%的浓硫酸(密度为1.84g/cm3)0.32ml,缓慢加入到适量去离子水中,配制成浓度为0.6M的硫酸水溶液;
(2)取步骤a中制备的沉积有Al-Pt二元合金的铝片,将样品的边缘和背面用有机漆进行封闭,留出面积为1cm2的Al-Pt二元合金表面,冷风干燥待用;
(3)在恒电位仪上进行阳极氧化:将封闭好的样品放入配制好的硫酸水溶液中并与电源的正极相连;将电源的负极与环形的纯铝片相连;采用饱和甘汞电极为参比电极;从开路电位(OCP)开始正向扫描至6V(OCP),扫描速率为33mv/s,制备出厚度约为110nm铂纳米颗粒负载介孔氧化铝,其微孔大小为12-25nm,铂纳米颗粒的大小为2-25nm。
实施例4
a、制备Al-Pt二元合金
Al-Pt二元合金的制备过程同实施例3中的a步骤。
b、制备铂纳米颗粒负载介孔氧化铝
(1)同实施例3中的b步骤中的(1)。
(2)同实施例3中的b步骤中的(2)。
(3)在恒电位仪上进行阳极氧化:将封闭好的样品放入配制好的硫酸水溶液中并与电源的正极相连;将电源的负极与环形的纯铝片相连;采用饱和甘汞电极为参比电极;在恒定电位3V(OCP)下进行阳极氧化20min,制备出厚度约为135nm铂纳米颗粒负载介孔氧化铝,其微孔大小为10-18nm,铂纳米颗粒的大小为3-18nm。
Claims (9)
1.一种铂纳米颗粒负载介孔氧化铝原位制备方法,其特征在于:包括如下步骤:
a、制备Al-Pt二元合金:在直径为5cm的纯铝靶材上缠绕2~5根直径0.5~1mm、长3~5cm的铂丝制成Al-Pt复合靶材;以铝片为基材,通过Al-Pt复合靶材和纯Al靶材双靶共溅射的方法制备Al-Pt二元合金;溅射电流分别为Al-Pt复合靶材110~200mA和纯Al靶200~320mA;溅射时间为10~20 min;
b、阳极氧化:将步骤a获得的Al-Pt二元合金置于0.3~0.6M的硫酸水溶液中,在0~6V动电位或恒电位阳极氧化,制备出铂纳米颗粒负载介孔氧化铝。
2.如权利要求1所述的方法,其特征在于:步骤a中在铝基材上获得一层厚100~200nm的Al-Pt二元合金,铂含量为1 at%~5 at%。
3.如权利要求1或2所述的方法,其特征在于:步骤b中在Al-Pt二元合金上制备出一层厚100~200nm的铂纳米颗负载介孔氧化铝,铂纳米颗粒的尺寸介于5~50nm,且均匀弥散的分布于介孔氧化铝的孔壁之中。
4.如权利要求1或2所述的方法,其特征在于:步骤a中,溅射电流分别为Al-Pt复合靶材110mA和纯Al靶320mA;溅射时间为10min。
5.如权利要求3所述的方法,其特征在于:步骤a中,溅射电流分别为Al-Pt复合靶材110mA和纯Al靶320mA;溅射时间为10min。
6.如权利要求1或2所述的方法,其特征在于:步骤b中硫酸水溶液浓度为0.4M。
7.如权利要求3所述的方法,其特征在于:步骤b中硫酸水溶液浓度为0.4M。
8.如权利要求1或2任一项所述的方法,其特征在于:步骤b中在3V电压阳极氧化20min。
9.如权利要求3所述的方法,其特征在于:步骤b中在3V电压阳极氧化20min。
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